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Phenyl acetone, Phenyl acetone in india, Phenyl acetone in bulk, best quality Phenyl acetone, Phenyl Acetone (1 Phenyl 2-Propanone), phenylacetone india, CAS NO.:103-79-7 - Phenyl Acetone – p2p, P2P, benzyl methyl ketone, phenyl 2 propanone, phenyl acetone manufacturers, phenyl acetone suppliers, phenyl acetone exporters, phenylacetone manufacturers, Manufacturers, Suppliers & Exporters, fine chemicals, MulBerry Chemicals Pvt. Ltd. Phenyl Acetone, 1 Phenyl 2-Propanone, manufacturers, CAS NO.:103-79-7, chemicals manufacturer India, supply, trade, export, manufacturing, fine chemicals, Intermediaries, phenylacetone, phenyl acetone, phenyl acetone chemicals, phenyl-2-propanone, benzyl methyl ketone, methyl benzyl ketone, buy, best quality, manufacturers, suppliers, exporters, mumbai, india, chemical, chemicals, p2p, P2P, chlorohexanone, 6 chlorohexanone, benzyl methyl ketone, phenyl 2 propanone, phenyl acetone manufacturers, phenyl acetone suppliers, phenyl acetone exporters, chloro hexanone, dibutyl ether, 1,4 dioxane, 6 methyl quinoline, 2 isobutyl quinoline, 6(8)secondary butyl quinoline, manufacturers, exporters, suppliers, mumbai, india Phenyl Acetone, 1-Phenyl 2-Propanone CAS NO.:103-79-7 - MulBerry Chemicals Pvt. Ltd high quality chemicals Phenyl Acetone, phenylacetone manufacturers, Di-n-butyl Ether, 1, 4 Dioxine, Quinoline and Substituted Quinoline and Grignard reagents etc. We are manufacturers, supplier, exporter of Phenyl Acetone chemicals in India, provides chemicals, p2p,benzyl methyl ketone, phenyl 2 propanone, phenyl acetone manufacturers, phenyl acetone suppliers, phenyl acetone exporters, chloro hexanone, dibutyl ether, 1,4 dioxane, 6 methyl quinoline, 2 isobutyl quinoline, 6(8)secondary butyl quinoline, manufacturers, suppliers and exporters in India.phenylacetone, phenyl acetone, phenyl acetone chemicals, phenyl-2-propanone, benzyl methyl ketone, methyl benzyl ketone, buy, best quality, manufacturers, suppliers, exporters, mumbai, india, dialnsearch Phenyl Acetone - Manufacturers, Suppliers and Exporters phenylacetone, (or phenyl-2-propanone, benzyl methyl ketone or methyl benzyl ketone. Often it's referred to as P2P) is an organic compound. It is a clear oil with a refractive index of 1.5168. This substance is used in the manufacture of methamphetamine and amphetamine as a starting material or intermediate. Due to the illicit uses in clandestine chemistry, it was declared a schedule II controlled substance in the United States
SYNTHESIS OF PHENYL-2-PROPANONE
Phenylacetone (known also as phenylpropan-2-one, benzyl methyl ketone, or methyl benzyl ketone), is an organic compound. It is a clear oil with a refractive index of 1.5168. This substance is used in the manufacture of methamphetamine and amphetamine as a starting material or intermediate, where it is commonly known as P2P. Due to the illicit uses in clandestine chemistry, it was declared a schedule II controlled substance in the United States 11 February 1980. Preparation There are many methods in the scientific literature to prepare phenylacetone, and due to its status as a controlled substance, there is crossover into popular literature such as works by Uncle Fester and Alexander Shulgin. Large amounts of data are available on the Internet relating to the preparation of phenylacetone. A conceptually simple example of phenylacetone organic synthesis is the Friedel-Crafts alkylation of benzene with chloroacetone.
Phenylacetone can also be produced from many other compounds. For example: phenylacetic acid is distilled with lead acetate or calcium acetate to yield phenylacetone. benzaldehyde is reacted with nitroethane yielding phenyl-2-nitropropene, which is reduced, usually in the presence of acid, to phenylacetone. Phenyl acetone is used as an intermediate to produce pesticides and anticoagulants. Active ingredients as anticoagulants include: Brodifacoum Chlorophacinone Coumachlor Difenacoum Diphenadione 2-Pivaloyl-1,3-indandione 2-Isovaleryl-1,3-indandione Warfarin 3,4-Methylenedioxyphenylpropan-2-one (MDP2P) is a chemical compound consisting of a phenylacetone moiety substituted with a methylenedioxy functional group. It is commonly synthesized from either safrole ((which, for comparison, is 3-[3,4-(methylenedioxy)phenyl]-1-propene) or its isomer isosafrole via oxidation using the Wacker oxidation or peroxyacid oxidation methods. MDP2P is a precursor in the chemical synthesis of the methylenedioxyphenethylamine (MDxx) class of compounds, the classic example of which is 3,4-methylenedioxy-N-methylamphetamine (MDMA), and is also an intermediate between the MDxx family and their slightly more distant precursor safrole or isosafrole. On account of its relation to the MDxx chemical class, MDP2P, as well as safrole and isosafrole, are in the United States (U.S.) Drug Enforcement Administration (DEA) List I of Chemicals of the Controlled Substances Act (CSA) via the Chemical Diversion and Trafficking Act (CDTA).
mumbai. manufacturers. phenylacetone india. Quinoline and Substituted Quinoline and Grignard reagents etc. Phenyl acetone in india. suppliers. phenyl acetone chemicals. benzyl methyl ketone. Phenyl acetone in india. but there has always sprung up new methods of performing the feat of making this compound. phenyl 2 propanone. phenyl acetone exporters. Suppliers and Exporters phenylacetone. buy.Phenyl acetone. best quality Phenyl acetone Phenyl acetone. export. phenyl acetone exporters. fine chemicals. We are manufacturers. p2p. exporters. dibutyl ether.:103-79-7. BMK. 6 methyl quinoline. phenyl acetone manufacturers. (or phenyl-2-propanone. ranging from simple one-step methods to elaborate multi-step variants. Phenyl acetone in bulk. benzyl methyl ketone.phenylacetone. use Phenyl acetone. P2P. It is a clear oil with a refractive index of 1. and also because of its popularity. phenyl acetone chemicals.5168
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Synthesis of Phenyl-2-Propanone (P2P) Table of Contents Table of Contents Introduction P2P from Benzyl Cyanide P2P from Phenylacetic Acid Friedel-Crafts Alkylation of Benzene with 2-Nitropropane Reduction of Phenyl-2-Nitropropene Friedel-Crafts Alkylation of Benzene with Chloroacetone Hydrolysis of Ephedrine Derivatives Electrochemical Coupling of Benzyl Chloride and Acetic Anhydride Nickel-mediated Coupling of Benzyl Chloride and Acetyl Chloride Semipinacol Rearrangement of Phenyl-2-Propanal P2P from Bromobenzene/Acetone Enolate Radical Alkylation of Benzene with Acetone. Benzyl Methyl Ketone or Phenylacetone). chlorohexanone. phenyl 2 propanone. benzyl methyl ketone. such as the ever popular MDMA precursor MDP2P (3. dibutyl ether. phenyl acetone suppliers. P2P. india.19 g/mol Density: 1.4 dioxane. Welcome to the world of P2P. Often it's referred to as P2P) is an organic compound.Phenyl Acetone – p2p. methyl benzyl ketone. 6 methyl quinoline. phenyl 2 propanone. This substance is used in the manufacture of methamphetamine and amphetamine as a starting material or intermediate. benzyl methyl ketone. Ltd. 6(8)secondary butyl quinoline. benzyl methyl ketone or methyl benzyl ketone. india.4 dioxane. the most popular precursor to amphetamine and methamphetamine is phenyl-2-propanone (also called P2P. phenylacetone. trade. exporters. 2 isobutyl quinoline. phenyl-2-propanone. There is an astounding array of synthetic routes to this compound. Here is a collection of some of the possible methods of synthesizing phenyl-2-propanone. and from the very easy to the very complicated. chemical. Manufacturers. phenyl acetone. Many of the syntheses can also be tweaked to produce substituted phenyl-2-propanones. chloro hexanone.0057 g/ml (20°C) Refractive Index: 1. 1-Phenyl 2-Propanone CAS NO. exporter of Phenyl Acetone chemicals in India. best quality. phenyl acetone. Suppliers & Exporters. 4 Dioxine. mumbai. 1. phenyl acetone manufacturers. Phenyl Acetone. phenyl-2-propanone. use Phenyl acetone.benzyl methyl ketone. supplier.:103-79-7 . 86-87°C/6mmHg Melting Point: -15°C Molecular Weight: 134.4-methylenedioxyphenyl-2-propanone) by using starting materials with the desirable aromatic substituents. phenylacetone manufacturers. methyl benzyl ketone. suppliers. Di-n-butyl Ether. exporters. Phenyl Acetone (1 Phenyl 2-Propanone). 6 chlorohexanone. phenyl acetone suppliers. 6(8)secondary butyl quinoline. catalyzed by Mn3+ Oxythallation of alpha-methylstyrene Wittig reaction of Benzaldehyde Cu(I)-catalyzed Arylation of Potassium Acetylacetonate Pd-catalyzed Arylation of Isopropenyl Acetate Alkylation of Benzyl cyanide with Trimethylaluminium P2P from Phenylacetaldehyde and Dimethyl Cadmium P2P from Phenylacetyl Chloride and Dimethyl Cadmium P2P via Grignard Addition to Acetic Anhydride P2P via Grignard Addition to Benzyl Cyanide References ----------------------------------------------------------------------------------------\ Introduction Aside from the often amateurish reduction of (pseudo)ephedrine to methamphetamine. suppliers and exporters in India. flowery odor Boiling Point: 214-216°C/760mmHg. Appearance: Clear oil. best quality. chemicals manufacturer India. provides chemicals. manufacturing. p2p. 1.:103-79-7 . dialnsearch Phenyl Acetone Manufacturers. 1 Phenyl 2-Propanone. CAS NO. mumbai. manufacturers.
after cooling. The mixture is thoroughly shaken. After all is added the flask is warmed on the steam bath until solution is complete and then for five minutes longer. The filter cake is practically colorless and corresponds 250-275g of dry sodium salt. originating from Russia. The oil and ether layers are washed successively with 100ml of water. the solution cooled to 0°C. and discarded. with vigorous shaking.3 liters of distilled water at room temperature. the temp being kept below 20°C (If pure dry alpha-phenylacetoacetonitrile is used. the condenser closed with a calcium chloride tube. The next morning the mixture is stirred with a wooden rod to break lumps. washed with ether. and kept at this temperature for two hours. 1750ml of water added rapidly.6 mol) clean sodium and 700 ml of absolute alcohol (dried over calcium oxide or sodium) in a 2000 ml round-bottomed flask equipped with a reflux condenser. Phenyl-2-Propanone2 350 ml of concentrated sulfuric acid is placed in a 3000ml flask and cooled to -10°C.2-1. The ketone forms a layer and. The sodium salt still wet with ether is dissolved in 1. half its weight of water should be added to the sulfuric acid or charring will take place on the steam bath).
. it weighs 125-150g (77-86% of the theoretical amount). The combined filtrates are placed in the freezing mixture until they can be worked up as indicated below.3 moles of dry product) is added slowly. and the nitrile precipitated by adding slowly. the ether combined with the oil and dried over 20g of anhydrous sodium sulfate. The fraction boiling at 110-112°C at 24 mmHg is collected.Phenyl-2-Propanone from Benzyl Cyanide
alpha-Phenylacetoacetonitrile1 A solution of sodium ethoxide is prepared from 60 g. The ether is removed from the filtrates. The precipitate separated by suction filtration and washed four times on the funnel with 250 ml portions of water. The moist cake weighing about 300g corresponds to 188-206g (59-64%) of dry colorless alphaphenylacetoacetonitrile. The total first crop of moist alpha-phenylacetoacetonitrile obtained according to the procedure above (corresponding to 188-206g or 1. To the hot solution added a mixture of 234g (2 moles) of pure benzyl cyanide 264g (3 moles) of dry ethyl acetate (dried by refluxing over P2O5 for 30min followed by distillation). The sodium sulfate is collected on a filter. with shaking. is separated and the acid layer extracted with 600ml of ether. and the flask placed on a vigorously boiling water bath and heated for two hours. 90 ml of glacial acetic acid. or 69-76% of the calculated mount. with occasional shaking. mp 87-89°C. cooled in a freezing mixture to 10°C. (2. The sodium salt is collected on a 6 inch Buchner funnel and washed four times on the funnel with 250 ml portions of ether. while the temperature is kept below 10°C. and the solution heated on the steam bath for two hours before standing overnight. A somewhat higher yield has been obtained by a different variation of this synthesis. The solution is cooled to 0°C. and the residue distilled from a modified Claisen flask with a 25 cm fractionating side arm.
the phenylacetone will condense with itself to form useless Dibenzyl Ketone. 0. Potassium Acetate/Copper Sulfate3c To a mixture of 136 g (1. The distillate will separate into two layers. After the addition of all the methyllithium the precipitate partly dissolved and a weakly opalescent solution was obtained. The excess of methyllithium was thus destroyed and lithium hydroxide was formed from the intermediate dilithium salt. pure product is collected at 100°C/15mmHg. Pyridine Method5 A mixture of phenylacetic acid (13. Methyllithium addition to Phenylacetic Acid27 In a 100ml rb flask equipped with a side tube for a gas inlet capillary.055 mole of an ethereal solution of methyllithium was added through the condenser. separated. Sodium Acetate Method (alternative)3b 50 g phenylacetic acid. To the residue there is added 400ml water and the mixture is extracted with 3x100mL dichloromethane (or chloroform). After separation of layers upper layer is removed and lower layer is three times decanted with water.5 g (56%) phenyl-2-propanone. just to create sufficient bubbles for stirring the solution during the experiment. bp 105°C/10 mmHg or 216°C at atmospherical pressure. making the synthesis more environmentally friendly. the rest is mixed with 1000 ml water after cooling down. and distilled. Removal of the solvent left a residue witging 12g.1 mol) anhydrous cupric sulphate is introduced 2000 ml anhydrous acetic anhydride in 4000 ml flask. a reflux condenser protected by a sodium hydroxide drying tube and magnetic stirring was placed 0.1 mol). and 16 g (0. A considerable improvement to this method has been made by Xtaldoc on a large scale. the solution was then refluxed for 10-30 minutes to complete the reaction. 70 g sodium or potassium acetate. Heating of the reaction mixture to 145-150°C on an oil bath provides sufficiently energetic evolution of carbon dioxide. CH2Cl2) is added and the mixture is poured to a flask containing 2000 ml icewater. A second distillation gives 50-55% yield of product boiling at 210-215°C at atmospherical pressure. Phenyl-2-Propanone Ketoxime was obtained in 88-90% yield. water was slowly added. dried (Na2SO4. Sodium Acetate Method (alternative)3b The Phenylacetic Acid (PAA). First an amount of water will distill. and the air was then expelled with a rapid stream of dry nitrogen. The mixture is refluxed 24 h. bp 120-140°C. The Lead(II)Acetate can be substituted with Calcium(II)Acetate. If necessary. The solution is dried over Na2SO4 and the dichloromethane is distilled off under ordinary pressure (and is saved for reuse) the rest of the volatiles are evaporated in vacuo. If the ratio is too small. the crude product is extracted with 2x250ml dichloromethane and the pooled organic layers are washed with cold diluted sodium hydroxide solution (any formed P2P enol ester must be hydrolyzed) until no more acids are present in the organic layer. The solvent is distilled off and fractionation column is placed on the top of the flask.Phenyl-2-Propanone from Phenylacetic Acid
In this reaction. which requires liberal application of heat. When all air had been expelled 0. CaCl2). Acetic Anhydride (AA) and Sodium Acetate (NaOAc) is put in to a large round-bottomed flask equipped with a reflux condenser fitted with a drying tube.0 mol) phenylacetic acid. the ether refluxed. which on fractional vacuum distillation gave 7. Remaining acetic acid and acetic anhydride is then removed. After removal of the solvent the residue was taken up in toluene and washed with 10% sodium hydroxide. Formation of the ketone is controlled by mixing an aliquot of the reaction mixture with excess of water and ammonium hydroxide until weakly alkaline – upon heating to boiling the oily layer must not disappear. Lead Acetate Method6 Place 1000g phenylacetic acid and 3000g anhydrous (or trihydrate) lead acetate in a distillation apparatus and heat. A vivid reaction took place. and a white precipitate was formed (lithium salt of the acid). The organic layer is separated and redistilled to give pure phenyl-2-propanone. The yield about 30ml (70%).026 mole (3. and the crude phenyl-2propanone is vacuum distilled at 25 mmHg.
. acetic anhydride (50 ml) and pyridine (50 ml) was refluxed six hours (in the beginning carbon dioxide evolution was vigorous. After the solution had reached room temperature. purify and reuse). The reflux setup is rearranged for distillation and excess solvent is removed (acetic acid and acetic anhydride.1mmHg. it is important that acetic anhydride is present in the reaction mixture in a large molar excess over the phenylacetic acid. 25 g anhydrous sodium acetate and 850 ml acetic anhydride are refluxed with stirring under moisture protection for 40 h. The solvent is stripped off under vacuum and by vacuum distilling at 125-135°C/30-32 mmHg the crude product is obtained.6 g. Yield 70-90 g (52-67%). After cooling 500 ml of solvent (CCl4. CHCl3. and next phenyl-2-propanone in this destructive distillation.5 g) of phenylacetic acid dissolved in 50 ml of ether. After 2-3 minutes the gas stream was slowed down. 500 ml acetic anhydride and acetic acid are distilled off. bp 30-64°C/0. which was distilled at 154-156°C/30mmHg.
After being warmed to ambient temperature (10-15 min). The 2. At the end of this period. About 300 ml of acid is needed.
. water (150 ml) was added and the resultant heterogenous mixture was stirred at reflux for 2h. Phenyl-2-nitropropene (10 g. but the acidity was confirmed with pH paper.65g (76%) of phenylacetone. When the generation of heat had subsided. which is then hydrolyzed by the acid into the desired phenyl-2propanone. the aqueous phase extracted with CH2Cl2. During the addition of H2O2/K2CO3 a white. the yellow solution was diluted with water (150 mL). After distillation of said oil at aspirator vacuum.1 mole) phenyl-2-nitropropene was dissolved in 200ml methanol in a 250ml Erlenmeyer flask situated on a magnetic stirrer. and the ethereal layer washed three times with half its volume of water. dried over Na2SO4. 7. a variety of the Nef reaction.1 mol. and the solvent removed under vacuum to give a clear yellow oil. Reduction with Iron Powder13 If phenyl-2-nitropropene is reduced by iron powder in an acidic medium (such as acetic acid or aqueous hydrochloric acid) the nitroalkene is reduced to the oxime.5 h.The alkaline water layer. usually pure enough for most purposes. Then. Reduction with Chromous Chloride18 Another method for reducing phenyl-2-nitropropene to phenyl-2-propanone in 80% yield is to use Chromium(II)chloride as the reducing agent. Triflic Acid Method14 A solution of 2-nitropropene (300 mg) in benzene (30 equivalents) was added to a well-stirred solution of CF3SO3H (10 equivalents with respect to 2-nitropropene) and benzene with the co-solvent of methylene chloride cooled to -40°C in a dry ice-acetone bath.7g) in dry CH2Cl2 (300ml) was added benzene (0. and the temperature was not allowed to to rise above 15°C. care being taken for the evolution of heat and CO2. neutralized with powdered NaHCO3 and saturated with NaCl. with good stirring. which can be a bit too thick for a weak magnetic stirrer to handle. and the mixture was refluxed on low heat for 1. 8. The ether solution was then dried over magnesium sulphate. and the pooled organic extracts washed with 1 M Na2CO3 solution and dried over MgSO4. The combined extracts was washed with 2x150 ml H2O and dried over MgSO4. The organic phase was separated.4 dinitrophenylhydrazone derivative. the yield was around 60-70% of phenyl-2propanone (P2P) as a light yellow oil. Titanium tetrachloride (0. recrystallized from methanol. After being stirred for 60 min (or when the starting material completely disappears on TLC). The reaction mixture was immediately (after 1 minute) poured into large excess dry methanol (100 mL) cooled to -78°C with vigorous stirring. The reaction mixture was poured into 2000ml water. so the mass can be stirred with a glass rod now and then during the first two hours. 100 ml of 30% H2O2 was then added.57 mol) in 140 ml HOAc. and the residue was flash chromatographed (on SiO2. together with 30 grams of anhydrous potassium carbonate. and the residue distilled under vacuum to give phenyl-2-propanone in 75% yield. Phenyl-2-Propanone from Phenyl-2-Nitropropene8 Sodium Borohydride/Nef Reaction In this preparation. Evaporation of the solvent followed by vacuum distillation (bp 100-101°C at 14mmHg) afforded Phenyl-2-propanone (ca 9g. after which the precipitate will be much looser and no match for any mag-stirrer. and the pooled organic extracts washed with 100ml 2M NaOH and 200ml H2O.1 mol. When the pH of the solution turned acid. the flask was once again placed in an ice/salt bath and the solution was allowed to cool to 0°C again. followed by hydrolysis of the nitro group with hydrogen peroxide and potassium carbonate. which contained the lithium salt of unreacted acid.5 mol. This synthesis is not suitable for ringsubstituted phenyl-2-nitropropenes.6g (0. filtered with suction. as the side chain tends to be oxidized when electron-donating substituents are present on the ring. 16. was removed in a separatory funnel. The solution was extracted with CH2Cl2. 392 mg (85%). The preparation is a one-pot synthesis.5-153. sticky precipitate forms. first at ordinary pressure and then at aspirator vacuum to give 2.2 mole) of NaBH4 was added a little at the time. the solution is slowly acidified with 2M HCl with good stirring. The mixture turned brownish and foamy. the ice/salt. All of the precipitate was also be gone at this point.5°C. Phenyl-2-propanone by nitroalkylation of benzene Titanium Tetrachloride Method7 To a stirred solution of 2-nitropropene (0. 70% of theory). eluting with CH2Cl2:n-hexane 12:7) to give pure phenyl-2-propanone. The solvent was distilled off. 39g) at room temperature. and the solution was left to stir for 18-24 hours at room temp. The next day. and chilled to 0°C with an ice/salt bath. the color became significantly more yellow. 61 mmol) was dissolved in 75 ml HOAc and slowly dripped into a refluxing slurry of Fe powder (32 g. without isolation of the intermediate. and concentrated. 19g) was then added dropwise into the mixture with stirring at the same temperature. filtered and the ether driven off. had mp 152. The solution was extracted with 3x100ml CH2Cl2. The organic phase was dried over MgSO4. 0.bath was removed and the solution was stirred at room temperature for two hours. and was extracted with 3x100 ml CH2Cl2.3g (0. as a colorless oil. phenyl-2-nitropropene is reduced to phenyl-2-nitropropane with NaBH4 in methanol.
the ether dried over anhydrous MgSO4 and the ether distilled on a steam bath. The use of a glovebox or bag is not required if contact of the lithium with air is kept to a minimum. decomposing the addition product with sodium carbonate solution. the solution was practically black.9 g (0.Phenyl-2-Propanone from Chloroacetone9 41 grams (0. Electrosynthesis of P2P from Benzyl Chloride4 Synthesis of phenyl-2-propanone from benzyl chloride (79 mmol) and acetic anhydride (686 mmol) by electrolysis of the reaction mixture. After distillation through a short vigreaux column. and naphthalene (0. phenyl-2-propanone is isolated by extraction with ether in 64% yield. 9-13 mmol). 0. metallic nickel which had adhered to the walls of the flask was scraped off with the stirrer and a magnet. All of the benzene solutions were combined and filtered. Another procedure33. After refluxing for 5 hours. and a mixture of appropriate reagents in glyme (10 mL) was then added to the nickel. 21-30 mmol). After the electrolysis using a current of 1A at a temperature of 0°C (2. are present in the solution. the cathode of nickel. the solvent is DMF (110g) and the supporting electrolyte is tetrabutylammonium fluoroborate (2 g. Metallic Nickel-Mediated Synthesis of P2P from Benzyl Chloride and Acetyl Chloride28. One piece of lithium with a shining metal surface was rinsed in hexane and transferred into a glass tube with a stopcock and a rubber septum which had been filled with argon. 20 ml of water and 20 ml of concentrated hydrochloric acid was added. and the reaction mixture was heated further to 145-150°C. The benzene layer was separated and the aqueous layer extracted with four 25 ml portions of benzene. The nickel precipitated as a bulky black powder in a clear colorless solution after standing. 130g (82%) of phenyl-2-propanone is isolated in a purity of 99. which then can be hydrolyzed into phenyl-2propanone and an amine salt. the remaining benzyl chloride. see the translation of the original patents. Phenyl-2-propanone from Ephedrine Derivatives10 When ephedrine and related compounds are heated in strong aqueous acid. The glass tube was evacuated to evaporate the hexane.29 Preparation of Metallic Nickel A 50-mL two-neck flask was equipped with a magnetic stirrer. and phenyl-2-propanone. Yield 6. Ephedrine derivatives that can be used in this procedure include Ephedrine. which is free from propiophenone. using a lead cathode and a carbon anode. The septum on the side neck was replaced with an addition funnel.5-3 hours the phenylacetone is steam distilled from the reaction mixture. the reaction equilibrium is driven towards the desired product by continuously removing the formed phenyl-2-propanone by the aid of steam distillation. 1025g 75% sulfuric acid was mixed with 1g ZnCl2. a rubber septum. 6 mmol). and the remaining viscous oil was distilled under reduced pressure. which spontaneously can rearrange to the isomeric imine (Schiff Base). and a condenser topped with argon inlet and outlet to oil pump. the reaction mixture was decomposed by slowly adding water through the condenser. filled with argon. and weighed.2 faradays per mole of benzyl chloride).16 mol) Ephedrine or Pseudoephedrine freebase was dissolved at a temperature of 50-100°C. The distillate was extracted with ether. At 125°C steam is passed through the solution to facilitate mixing of the contents. The phenyl-2Propanone was distilled under reduced pressure. and during 2. The anode is made of magnesium or aluminium.1 equiv.31 mole) of anhydrous aluminum chloride and 100 ml of anhydrous benzene (free from thiophene) were put in a 500ml three-necked flask which was equipped with a mercury-sealed stirrer. Lithium metal was cut under mineral oil. Norephedrine and Norpseudoephedrine (Phenylpropanolamine). Many other metal salts can be used instead of the zinc chloride. Then. The top of the condenser was connected to a sulfuric acid trap and this trap was connected to a gas absorption bottle. Pseudoephedrine. bp 108-114°C/20-22mmHg. stirring during the addition. Approximately 10g of high-boiling material was left in the distilling flask. After the lithium metal was consumed completely. DMF as the solvent and a tetrabutylammonium tosylate electrolyte gives a 73% yield of phenyl-2-propanone after hydrolysis of the resulting enol ester. they are dehydrated to the enamine. the stirring was stopped.8%. both in free form and in the form of its enol acetate.5 g (32%).15 mole) of chloroacetone was allowed drop in slowly during a period of 30 minutes. is isolated by toluene extraction of the distillate. Nickel halide (1. the toluene which is a byproduct of the reduction of benzyl chloride. and 192g (1. lithium (2. During the reduction the surface of lithium became pink. The benzene was distilled off. for details.3 mmol) were placed in the flask through the side neck. glyme (25-30 mL) was added through the septum with a syringe. The the crude phenyl-2-propanone.0 equiv. After the DMF has been evaporated off and the residue has been hydrolysed with hot dilute HCl.9-1. a reflux water condenser and a small addition funnel. and the mixture was stirred for 12 h. filtering. and steam distilled as long as any oil distilled over. The flask was evacuated and filled with argon two or three times.
. Phenyl-2Propanone was recovered from the distillate by making the bisulfite addition product. At 145°C the stream of steam is increased.3 equiv. The mixture was stirred and heated to refluxing on a steam bath and 13. After cooling to room temperature. As all the steps are reversible processes. When no more hydrogen chloride was evolved. Nine grams of liquid boiling below 123°C/20-22mmHg was obtained.
bp 95-96°C (11 mmHg). bp 92-101°C at 14mmHg. When the ice has melted. The combined extracts were dried over anhydrous sodium sulfate and concentrated. the ether distilled off and finally the residue is vacuum distilled (bp 91-96°C at 11 mmHg) to give 5. The oily residue is then vacuum distilled with a fractionating column to collect the phenyl-2-propanone in a yield of 80% or more. 2Phenylpropionaldehyde. and is not disastrous for your health or the environment. Fractional distillation could theoretically be used to separate them. 8. 60g of mercuric chloride contains 45 grams of mercury. 7.122 g. and if you happen to ingest it yourself.9 mmol) and acetyl chloride (0.152 g. alpha-methyl benzeneacetaldehyde and alpha-methyl phenylacetaldehyde. the organics are extracted from the water phase by 3x50ml diethyl ether. 0. the pooled organic phases dried over MgSO4. It was eluted with hexane followed by chloroform to give phenyl-2-propanone (0. The chloroform solution was washed with water. The distillate is extracted with ether. and then the mixture is poured onto crushed ice (100-150g is probably a suitable amount). It is not possible to effectively separate 2-phenylpropanal (bp 222°C/760mmHg) from phenyl-2-propanone (bp 214°C/760mmHg) through simple distillation and certainly not via vacuum distillation as the boiling points are too close. only 10% phenyl-2-propanone was formed. poured into a separatory funnel containing hydrochloric acid solution (37%. A mixture of benzyl chloride (1. Additional heating was continued for 15 min. and naphthalene (0. A good idea for separating a mixture of the two is to oxidize the mixture with a mild oxidant which won't affect the P2P.Reaction of Benzyl Chloride with Acetyl Chloride in the Presence of Metallic Nickel Metallic nickel in glyme (25 mL). Method B 9 g of 2-phenylpropanal is slowly added with good stirring during 35 minutes to 40ml concentrated sulfuric acid.72 g. dried. Cumenealdehyde. The crude oil was purified by silica gel chromatography. Water is added. After all the 2-phenylpropanal has been added. I would definitely reccommend the one with sulfuric acid. and the solution is steam-distilled (during which operation the precipitate redissolves). There are other ways of performing this rearrangement. The P2P stays in the organic layer. followed by condensation of the vapors and redistilling the P2P12.9 mmol). The CAS number for 2-phenyl-propanal is [93-53-8]. and the red-brown reaction mixture was cooled to room temperature. 222°C/760mmHg. the mixture is allowed to stand at the same temperature for another 15 minutes. it will accumulate in your body. Phenyl-2-Propanone by Rearrangement of 2-Phenylpropanal11 2-Phenylpropanal can be rearranged with either mercuric chloride (HgCl2) or sulfuric acid (H2SO4) to form the isomeric phenyl-2-Propanone (P2P). 2-Phenyl-propanal (hydratropic aldehyde) is an unwatched industrial chemical which is used in the perfume industry. and extracted with chloroform twice. The acid can then be separated from the ketone by dissolving the mixture in a non-polar solvent and washing the solution with dilute sodium hydroxide. and the solvent is evaporated. enough to poison a medium-sized lake if released into the environment. during which time a precipitate forms.65 g.1 equivalents of HgCl2 was used.5h at 100°C in a boiling water bath. and the aqueous phase was extracted with additional chloroform. 2-phenylpropanal is isomerized to phenyl-2-propanone in up to 87% yield by passing its vapor over an iron zeolite catalyst bed at 500°C.6g (62%) of phenyl-2-propanone. the rest consisted of unchanged aldehyde. as it is much cheaper to use. lithium (0. When 0.0 g. IR (neat) 1710 cm-1 (C=O).3 mmol) in glyme (10 mL) was added dropwise for 30 min.95 mmol). while the temperature of the reaction mixture is kept at -16°C. prepared from nickel iodide (2. but which will oxidize the aldehyde to 2-phenylpropionic acid.) and 450ml 75% ethanol in a pressure-safe sealed glass container for 4. 21. Method A 30g of 2-phenylpropanal is heated together with a mixture of 60g mercuric chloride (HgCl2. 100 mL).
. but the size of the column that would have to be used makes that option impractical. which is then dried over MgSO4. 2-phenylpropanal can also be made from alpha-methylstyrene. 68%).97 mmol). and synonyms for it include Hydratropic aldehyde. Boiling point 92-94°C/12mmHg. was heated to reflux. the solvent removed under vacuum and the residue vacuum distilled to give pure P2P. 1 eq. Even if the method below which uses mercuric chloride is higher yielding than the one using cold sulfuric acid.
alpha-Methylstyrene can also be treated with Bromine and Sulfuric Acid to yield P2P.30 mol) in 125 mL benzene. acetone (150ml) and glacial acetic acid (250ml) was refluxed under an inert atmosphere (argon.34g) based on the reacted manganese(III)acetate. The yields in the reactions range between 50 and 98%.4g.29 mol) and alpha-chloroethyl methyl ether16 (28. dried over MgSO4 and the solvent distilled off. Thallium(III)Nitrate (mol wt 390) is stable indefinitely if stored in tightly sealed bottles. The ylid resulting from treatment of the phosphonium salt with base was found to be very unstable at room tempature. 100 mmol) in 100ml methanol is added to a solution of alpha-methylstyrene (11. and there is an immediate precipitation of Thallium(I)Nitrate. and the reaction is also applicable for other substituted benzenes. Potassium tert-butoxide (33 mmol) in 15 mL of glyme was added with stirring over 5 minutes. washed with a little methanol. The ether layer was separated and washed with 250ml water and with 2x250ml 5% Na2CO3 to remove any remaining acetic acid. Accordingly. the solvent evaporated and the residue fractionately distilled to recover unreacted benzene.Phenyl-2-Propanone from Acetone Enolate If acetone is reacted with a strong base. and after standing for 15 minutes. The salt is readily soluble in methanol and dilute mineral acids. and may be lethal upon ingestion! Handle with gloves only! A solution of Thallium(III)Nitrate (39g. but other ketone enolates. as can be seen in the comprehensive Manganese(III)acetate catalyzed aromatic acetonylation document on this site.2-propanone. and the residue vacuum distilled to give 10. The reaction can be catalyzed by iron salts. 50 mmol). such as pinacolone has been extensively studied in this medium. The reaction relies upon the special oxidative powers of manganese(III)acetate.4g. Phenyl-2-Propanone by Oxythallation of alpha-methylstyrene with Thallium(III)Nitrate23 Warning: Thallium salts are exceedingly toxic. lithium diisopropylamide and several alkoxides. The solution is extracted with ether.0 Free-Radical alkylation of Benzene with Acetone Catalyzed by Manganese(III)Acetate17 Phenyl-2-Propanone can be made in a single step by a free-radical reaction between benzene and acetone. the two species will combine to form phenyl. 88%) consisting of the crude phosphonium salt containing one molar equivalient of benzene crystallization. The ether was then dried over anhydrous Na2SO4 (or MgSO4). After standing for 40 h the mixture was filtered and washed with ether giving a white solid (112g. oxygen or UV light. but bromobenzene should also work) in DMSO under rigidly anhydrous conditions.
. but this can be improved. helium or nitrogen) until the dark brown color of manganese(III)acetate changed to the pale pink of manganese(II)acetate (about 90 min). There has been no known actual attempts at this synthesis using the enolate of acetone and a halobenzene in DMSO (but it has been done in liquid ammonia). a compound easily prepared from potassium permanganate. There are no theoretical obstacles at all to why it would not work in the production of phenyl-2propanone. the precipitate is filtered off. This salt is slightly hygroscopic on exposure in air but can be stored indefinitely in a sealed container. and requires high dilution of the reactants. The colorless crystals of Thallium(III)Nitrate trihydrate are filtered. and the filtrate is shaken for 5 min with 1M H2SO4 to hydrolyze the formed Phenyl-2-Propanone dimethyl acetal. benzene (150ml). the preparation and reaction of this ylid was best carried out at -40°C. read Drone #342's Enolate Phenylacetone Synthesis FAQ 1. acetone enolate is formed in quantitative yield. the characteristic red color dissappearing within a few seconds. which is able to deprotonate one of the relatively acidic alpha protons of the ketone.9g Phenyl-2-Propanone (81% yield). 100mmol) in 50ml methanol at room temperature with stirring.4g. Such strong bases include sodium amide. for example potassium tert-butoxide. and to give phenyl-2-propanone in 40% yield (1. The mixture was allowed to warm to room temp over 1h and was then directly distilled. For a more in-depth discussion of this synthesis. At this point a solution of benzaldehyde (30 mmol) in 5 mL of glyme was added over five minutes. The reaction mixture was partitioned between 400ml ether and 250ml water. The phosphonium salt (33 mmol) was suspended in 40 mL of glyme at -40°C under nitrogen. If this enolate of acetone is allowed to react with a halobenzene (preferably iodobenzene. washed with a little dilute nitric acid and dried in vacuo over phsphorus pentoxide. Thallium(III)Nitrate 50g Thallium(III)Oxide (Tl2O3) is dissolved in 150ml warm. concentrated nitric acid and cooling the pale yellow solution to 0°C.82g. 0. A mixture of Manganese(III)acetate dihydrate (13. The yield is relatively low. Phenyl-2-Propanone from Benzaldehyde and a Phosphonium Ylide (Wittig reaction)15 The phosphonium salt was prepared by dissolving triphenyl phosphine (76. which is the limiting reagent in this reaction. 0. to give pure phenyl-2-propanone enol methyl ether).
freshly distilled phenylacetaldehyde (Note 1) and 50 ml.75g of crude phenyl-2-propanone as an oil. which can be purified by vacuum distillation or column chromatography. Be prepared to stop addition and cool if needed. bp. isopropenyl acetate (9g. 167 mmol) and potassium acetylacetonate hemihydrate (125g. of halide ether solution to enter flask. and extract water layer with 2x50 ml portions of technical grade ether. under nitrogen. Do not add more! Take a glass rod about 12 inches in length and score with a 3 corner file 2 inches from one end using pliers and a rag to protect your hands break away the 2 inch piece. When all the halide has been added and the reaction is no longer refluxing. Add dropwise the aldehyde/ether solution to the dimethyl cadmium swirling occasionally to break up the clumps.67 mmol) in dry toluene (30 ml). 100 at 13 mm. The organic layer was washed with aqueous NaHCO3. The residue was chromatographed on silica gel. dried over magnesium sulphate and concentrated in vacuo to leave a dark brown oil. Phenyl-2-Propanone To a clean dry sep. Test with bisulfite any product not forming addition is phenyl-2-propanol (very small amount) can be saved for later oxidation. Quickly pour into a 1000 ml. After all the Cadmium chloride has been added. Add 60 ml. The solution was heated to boiling and the solvent was then evaporated to give relatively pure phenyl-2-propanone in 88% overall yield. Yield 50-55 ml. methyl iodide either freshly prepared or dried overnight with calcium chloride. Aldrich). 90 mmol. The mixture was stirred and heated at 100°C for 5 hr. 90 mmol) and dichloro-bis-(tri-otolylphosphine)palladium (0. Proceed immediately to next part if at all possible. Attach 125ml sep. add 31. was added tributyltin methoxide (25. 834 mmol.3 ml. Phenyl-2-Propanone from Benzyl cyanide and Trimethylaluminum25 Trimethylaluminium (30ml of a 2M solution in toluene) was added to a solution of benzyl cyanide (2. ~85% of P2P. sodium bicarbonate. Add 12. If cloudiness does not become apparent in 1 or 2 min stop. Be prepared to stop and cool with ice water bath if needed. Notes: Avoid breathing the cadmium chloride dust (it needs to be finely ground after drying) avoid contact with the methyl iodide or ether solution of methyl iodide avoid breathing any vapours of the metal conversion reaction (it smells like garlic if you must know).2 grams of anhydrous cadmium chloride in small portions through side neck restoppering after each addition.Phenyl-2-propanone was conveniently prepared from the enol ether by mixing with one equivalent of water with 0. distilled water 10 ml conc. 20 mmol) in 20ml of toluene at -78°C and the mixture was under stirring allowed to slowly warm up to room temperature and refluxed for 12h. Add 75 ml anhydrous ether to flask. 10 ml. add halide dropwise as quickly as the reflux column can handle.4g. to afford the phenyl-2-propanone in 67% yield. which after purification gave phenyl-2propanone in 65% yield. funnel. keep it covered and protected from air. When reflux has subsided do not heat. The combined extracts were washed with water. 3-neck rb. replace stopper. Phenyl-2-Propanone by arylation of Potassium Acetylacetonate21 To a stirred solution of bromobenzene (31.47g.9 ml.5% HCl and enough methanol to effect solution.
. DRY FLASK attach a reflux condenser. beaker containing 100 ml. using the remaing 10 inch piece gently poke at the magnesium turnings to expose fresh metal. HCl and 100 cc. The mixture was stirred and heated at 100°C for 24 hr. stirred with 2M sodium hydroxide (250 ml) for 1 hr and extracted with toluene (2x500 ml). 0. Removal of the solvent gave 2. Phenyl-2-Propanone from Phenylacetaldehyde and Dimethyl cadmium Dimethyl Cadmium 2 MeMgI + CdCl2 => Me2Cd + 2 MgICl To 500 ml. Hydrolyse addition product and distill if desired. add 31.4 g. This polymer is degraded to the monomer on distillation. 200 mmol) in DMF (1 liter) was added cuprous iodide (32. Allow aprox. Phenyl-2-Propanone by Heck Arylation22 To a stirred solution of bromobenzene (60 mmol). Note 1: The phenylacetaldehyde will polymerise on standing. Neutralize with sat. funnel add 64 ml. aq. Ethyl acetate was added and the mixture was vigorously stirred for one hour. Aldrich). the flask will have a tannish brown solid mass inside. cooled and the solvent evaporated in vacuo. Distill under reduced pressure to strip off excess ether. brine and dried over MgSO4. For this preparation it also needs to be as dry as possible. If reaction starts. anhydrous ether. funnel. This is the dimethyl cadmium.34g. of chipped ice. 1M hydrochloric acid and satd. the solution was poured over crushed ice and made acidic with 6M HCl. Separate. sodium bicarb untill fizzing stops. cooled. After being cooled to 0°C. anhydrous diethyl ether to sep.5 grams Magnesium turnings to flask.
2 mol) and magnesium shavings (4. and refluxed on a steam cone for 1 hour. about 75-80% of the theoretical 26 ml. 0. but as it began to turn yellow. NaCl was added to the aqueous layer. which was then extracted w/Et2O [NOTE: I think a lot of product was left behind in this aqueous layer. followed by 50 ml brine. dried over MgSO4. 52%). then another 10 ml (The complex reacted immediatly with the water. of anhydrous benzene and the distillation was continued until about 50 ml.9 grams (0. stirring under reflux was continued for an additional hour. as theoretically expected by a substance having a melting point at -16. The aqueous layer was separated.24 127g benzyl chloride was dissolved in 250mL Et2O. corresponding to a intermediate complex. of anhydrous ether and 6. the cooling bath removed and the reaction quenched by the careful addition of saturated aqueous ammonium chloride.Phenyl-2-Propanone from Phenylacetyl Chloride and Dimethyl Cadmium32 A mixture of 40 ml. Again 100 ml of anhydrous benzene was added. then left to cool to room temp.) The solution was exposed for a vacuum to remove any remaining ether in the solution.2 mol benzylmagesiumchloride grignard reagent were prepared by standard methods in diethylether (Total reaction volume: 200ml). 2. then acidified.5g. The reaction mixture was warmed to room temperature and refluxed with stirring on a steam cone for 1 hour. filtered. I think the purity of final product would be higher if reaction mixture was first poured onto ice. warmed to room temperature. it was still very orange even after adding NaCl and extracting with Et2O (which was a lighter shade of orange than the aq. A white percipitate was formed. and no further reaction occurred.25 mole) of magnesium was stirred under reflux while 35. The white complex was briefly dried. About 2 moles of acetonitrile (100ml) was mixed with 100 ml of anhydrous diethylether and cooled in ice/water.4 grams (0.2 mole) of phenylacetyl chloride in 75 ml of anhydrous benzene was added with stirring over a period of approximately 10 minutes.to 10-minute period. After completion of addition. stirred thoroughly.9g. After the addition after one hour was finished. This method could be of interest for producing P2P from acetonitrile. layer!)].1 grams (0. A thick white precipitate built up and clogged up some Mg. of 62g acetonitrile in 100mL Et2O was added slowly while stirring w/a thermometer. not soluble in ether or acetonitrile. the organic phase washed with 10% sodium carbonate solution until the washes were no longer acidic to universal pH paper.Submersion of the flask in cold H2O was used as necessary during addition to prevent excessive boiling of the Et2O. The benzylmagnesium chloride solution was added the acetonitrile over a periode of 10 minutes. by Poodle: In a dream. This complex was isolated by filtration through a buchner. bp 214-215°C/760mmHg (100-101°C/13mmHg). so try to avoid it!]. the ether evaporated on a water bath and the residue fractionately distilled to yield phenyl-2-propanone (14g. Phenyl-2-Propanone by Grignard addition to Nitriles19. a thermometer and an addition funnel (modified so that the added liquid was cooled externally by dry ice/acetone). Ether was removed by distillation on a steam bath. A soln.
. [NOTE: This clogged-up material didn't react fully w/the MeCN.5 grams (58%) of 1-phenyl-2-propanone. To this was added an etheral solution of benzylmagnesium chloride. no chances was taken and 15 ml distilled water was added.] After all effervescence had stopped. to this was added 27g Mg turnings in portions. 500mL 10% HCl was added slowly under stirring. The flask was again cooled in an ice bath and the reaction mixture decomposed by the addition of a solution of 25 grams of ammonium chloride in 200 ml of cold water. [NOTE: This seemed to cause the Et2O layer to take on a reddish tint. The intermediate phenyl-2-propanone imine magnesium salt can also be prepared from methylmagnesium iodide and benzyl cyanide. of anhydrous ether was added over a 3-hour period. The organic phase was separated. more of distillate was collected. The reaction mixture was cooled with an ice bath and 22. The combined Et2O layers were washed with H2O. The ketone was frozen at -20. The benzene was removed by flash distillation and the ketone distilled under reduced pressure. Upon using the vaccum. Vacuum distillation of this oil afforded pure phenyl-2-propanone (bp 91-96°C at 11 mmHg). Phenyl-2-Propanone by Grignard Addition to Acetic Anhydride26 In a 500-mL three-necked flask. and dried over anhydrous sodium sulfate.55 mol) in diethyl ether (100ml). To theresidue was added 100 ml. an iodine crystal being added after the first portion to initiate Grignard rxn. washed. there was excess unclogged Mg which would not react. The organic phase was dried over MgSO4. The imine salt can also be reduced directly to amphetamine by sodium borohydride in methanol in high yield. The reaction temperature rose to 30°C. there was added a solution of acetic anhydride (40g. 0. the organic layer was separated. the mixture was refluxed gently.2 mol). Et2O and a small amount of toluene were evaporated to give 42g crude phenyl-2-propanone as a clear orange oil. Reaction initiated by heating the mixture to 60°C for a short periode of time.25 mole) of methyl iodide in 140 ml. and washed twice with water-free ether to remove any unwanted remains of acetonitrile or benzyl chloride. There was thus obtained 15. The oily layer was separated and gave 21 ml of possible P2P. ether was removed and the solution separated into two layers with an orange oil on top and a water layer containing salts and undissolved salts. bp 74-76°C/3 mmHg).134 mole) of powdered anhydrous cadmium chloride was added over a 5.5 grams (0. 0. Both are hydrolyzed to phenyl-2-propanone with dilute hydrochloric acid. the reaction mixture was allowed to stir at dry ice temperature for 2-3 hours. the rxn mixture was cooled in an ice-salt bath. and the flask was equipped with a magnetic stirrer. After all Mg was added. as it greatly simplifies the procedure by eliminating any need for extensive extraction of the ketone. and so was decomposed to toluene. the flask was cooled in an ice bath. situated in a dry ice/acetone slush in a Dewar flask. the solution turned yellow/orange with oily orange bubbles. prepared from benzyl chloride (25. Simplification of the above procedure. giving heat and causing remaining ether to boil. responding to that temperature by forming a solid. and 30. but after all was added. using constant swirling of the reaction mixture.
Ohwada. 21. Lett. 1975 (1960) Chem. 49. 68. Practical Organic Chemistry.. 2112 (1935) Juraj Kizlink. References Org. 612-613. Lett. T. 471). 11(4) 339 (1941). 54. Chem. 993-4 (1990) US Pat 4. Lett. K. Shudo. (bp 91-96°C at 11 mmHg).2 mol benzyl chloride in 100ml anhydrous ether and 0. and was allowed to stand without drying overight. Org. Ohta. Using benzyl cadmium chloride or dibenzyl cadmium gave little difference in yield. K.026. Vol. K. Chem. 45. The ether layer was separated and the aqueous phase extracted twice with ether. 225. Tet.694. Zh. Chem.232 Danilov and Danilova. Chemicke Listy 84(9). Chem. 3323-3326 (1964) Ann. K.541 [ Reference Lost ] A. I. Synthesis 723-726 (1994) J. if the ratio was less a considerable amount of acid was found in the product. and the residue vacuum distilled to give phenyl-2-propanone in 50-70% yield (calculated on the acid chloride).16 mol) was added with vigorous stirring over 10-15 min. 597-600 (1982) Bull. T. 7539-7555 (1990) D. The ether solution was then extracted with 4x25ml 10% sodium bicarbonate. R. 1603-1607 (1984) Tet... Syn. T. Chem.1 mol acetyl chloride in 3 volumes anhydrous ether was added to the cold benzyl cadmium reagent over 5 min.200. Coll.30. 60. Abs.. 2. Coll. Coll. 1622 (1940) German Patents 3. Soc. Am. 5th Ed. Ber. Org.2 mol per 300ml and then cooled in an ice-bath. A new Synthesis of Methyl Ketones. Vol 1. The solution of the grignard reagent was diluted with ether so that the concentration was no greater than 0. and hydrolyzed with 20% H2SO4. 5868 (1941) Chem. Tet. Chem. The combined ether solutions were washed with water and 10% sodium bicarbonate. Ber. Vol. 60.. Soc. 269 (1884) J. so keep it on ice during handling. 2.107 Alexander Shulgin. McKillop. p 487-489 Org. Tet. 2977-2978 (1988) R. p. p. Khimii. Amer. Jap. 155-158 (1980) J. 62. The mixture was stirred in an ice-bath for 8h. 29(24).452. Lett. and the combined aqueous extracts were extracted twice with ether. Lett. 26.Phenyl-2-Propanone from Benzylchloride (via dibenzyl cadmium)20. A solution of 0. It was necessary to use a 2:1 molar ratio of the cadmium reagent to acid chloride. The ether was distilled off. 733 (1989) Okabe. Anhydrous cadmium chloride (0. A. Vogel. Lett. Oxidative Rearrangement of Olefins with Thallium(III)nitrate. 1050 (1927) US Patent 4. Stirring was continued with cooling for 2h. 5275-5280 (1970). p 391-392 Magidson and Garkusha.2 mol magnesium turnings (Org. 242 (1984) A. The thermal stability of dibenzyl cadmium is low. Ohta. Syn. and all the pooled ether extracts were washed with water and dried over sodium sulfate. Synth. Ohwada. H. Obsh. Pihkal #109 Okabe. Tetrahedron 46. US Pat 3. Chem. Soc. 3777 (1985) Tet. T.31 2 PhCH2MgCl + CdCl2 → (PhCH2)2Cd + 2 MgCl2 (PhCH2)2Cd + 2 CH3COCl → 2 PhCH2COCH3 + CdO Benzylmagnesium chloride was prepared from a solution of 0. J.. Chem. 82. Oxidation of Olefinic Compounds with Solutions of Thallium(III) Salts.047
. The clear dark solution was filtered under nitrogen through a glass wool plug. 57. Frye. Ballini. Shudo. Coulsen.698 and 3.629.
Rec. With prime focus on quality. Chem. T. 6. 1373-1381 (1985) Tet. benzyl methyl ketone or methyl benzyl ketone (Phenyl-2-propanone / Benzyl methyl ketone). dyes. Hirashima and J. F.639. Engineering Data 15(1).
. Alkyl Benzyl Ketones and Hydantoin Derivatives.780 J. Due to the illicit uses in clandestine chemistry. Sund and H.H.4-methylenedioxy phenyl-2-propanone) which is used in the clandestine synthesis of MDMA (3. We are one of the leading manufacturers of fine chemicals. phenyl isopropyl amine. Nelson. Lett. Amer. Phenylacetone is called MDP2P (3. fungicides. 1-phenyl-(103-79-7) Benzyl methyl ketone(103-79-7) C9H10O 1-PHENYLACETONE1-PHENYL-2PROPANONEBENZYL METHYL KETONEPHENYLACETONEPHENYL-2-PROPANONE1phenyl-2-propanon1-phenyl-propan-2-one2-Propanone. Chemistry Letters 2005-2008 (1991)
Phenyl acetone is used as an intermediate to produce sympathomimetic amines such as phenbenzamine. biocides. pargyline and estramustine. commonly known as ecstasy. February 1980.
Phenyl acetone family compounds are widely used as a parent compound to make drugs. Chem. J. 3369-3370 (1972) US Pat 5. Soc. Phenylacetone is called MDP2P (3. 154 (1945) Acta Chem. 741 (1939) H. Phenylacetone shipment is available only to the importer who has import licence issued by Government. Phenylacetone shipment is available only to the importer who has import licence issued by Government. phenyl isopropyl amine. 782-790 (1952) J. Chromatography. methyl benzyl ketone. Oki. commonly known as ecstasy. 200-201 (1970) I.4methylenedioxymethamphetamine). Often it's referred to as P2P) is an organic compound. suppliers & exporters of phenylacetone.4methylenedioxymethamphetamine). phenylacetone is also called phenyl-2-propanone. Analytical and many others. and flavoring agents. Chem. Scand. 50. rubber chemicals. Technical Service: Our team of scientists has experience in all areas of research including Life Science. prenylamine. prenylamine.5168. amphetamine.. benzyl methyl ketone. 518-530 (1936) E. it was declared a schedule II controlled substance in the United States 11. Soc. Org. Chim. Chem. Bulk Ordering & Pricing: Need larger quantities for your development. 61. T. It is clear oil with a refractive index of 1. We accept the complete responsibility for the process and quality aspects of each and every product we offer. J. pargyline and estramustine. Chemical Synthesis. Electroreductive Acylation of Benzyl Chlorides with Acid Anhydrides. Org.R.4-methylenedioxy phenyl-2-propanone) which is used in the clandestine synthesis of MDMA (3. Trav. 37. alkaloids. 67. This substance is used in the manufacture of methamphetamine and amphetamine as a starting material or intermediate. amphetamine. We are leading Manufacturers and exporters of phenylacetone. Gilman. 24. 55. manufacturing or research applications? Phenyl acetone is used as an intermediate to produce sympathomimetic amines such as phenbenzamine. 2451-2452 (1983) J.J. This commitment to quality and the obligation to our customers have been the foundation of our business since its inception. phenylacetone is also called phenyl-2-propanone. Shiokawa. . Am. Material Science. Chem. we have adopted high level of operational quality standards that are strict on both the domestic as well as international market grounds. Henze. Nishiguchi. Often it's referred to as P2P (C9H10O) is an organic compound.
phenyl isopropyl amine.3-indandione Warfarin Note: Reproduction of any materials from the site is strictly forbidden without permission. Phenylacetone shipment is available only to the importer who has import licence issued by Government. Phenylacetone is called MDP2P (3. Active ingredients as anticoagulant include: Brodifacoum Chlorophacinone Coumachlor Difenacoum Diphacinane 2-Pivaloyl-1. Phenyl acetone is used as an intermediate to produce pesticides and anticoagulants.4methylenedioxymethamphetamine).Phenyl acetone is structurally related to coumarine or cinnamic acid for the application of rodenticide anticoagulant and to phenethylamine which is a main structure in the activity of the sympathetic nervous system. Other use as an intermediate in the manufacture of Amphetamine Prenylamine Pargyline Estramustine Chlorophacinone & Diphacinone (rodenticides)
.4-methylenedioxy phenyl-2-propanone) which is used in the clandestine synthesis of MDMA (3. prenylamine. CAUTION : PHENYL ACETONE MAY BE A CONTROLLED COMMODITY IN YOUR COUNTRY Phenyl acetone is used as an intermediate to produce sympathomimetic amines such as phenbenzamine. commonly known as ecstasy.3-indandione 2-Isovaleryl-1. amphetamine. pargyline and estramustine.
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© 2009-2011. Ltd ("Mulberry Chemicals") or an affiliated company of MBC. Dist.1019.D.18 g mol. MulBerry Chemicals Pvt. Ltd in India.Sarigam. Plot No.
Contact information for MulBerry Chemicals Pvt.C.006 g/mL -15 °C. 487-489 K.Valsad.Phenylacetone
Other names benzyl methyl ketone. G. Road No. 5 °F 214-216 °C. . . 10. methyl benzyl ketone.
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The above information is believed to be correct but does not purport to be all-inclusive and shall be used only as a guide.1 1. Ltd .I. phenyl-2propanone Identifiers CAS number 103-79-7 PubChem 7678 ChemSpider 21106366 UNII O7IZH10V9Y KEGG C15512 ChEBI CHEBI:52052
Molecular formula Molar mass Densit y Melting point Boiling point
Properties C 9H10O 134. .