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......there is the option to turn your recemic amphetamine to d-amphetamine in w hich case it's not hydroscopic ....

a problem associated mainly with the recemic amphetamine......the recemic amphetamine free base is treated with tartaric acid to salt the l- out as the amphetamine tartrate and the liquid remaining is the d-amphetamine...which is ph to 13 to free the d-free base oil, then extracted wi th toluene and gassed....mp of d-amphetamine is 156C......prove the statement wr ong, also shards can be made of the material the usual way.....solo Read more: http://www.drugs-forum.com/forum/showthread.php?t=21645#ixzz1mybP1SWZ well protected. The instructions to make chloroform are listed in an easy-to-fol low bulleted list: Start by filling up a glass container with half a liter of bleach Lower the temperature of the bleach solution by adding ice also into the contain er and allowing it to cool. Pour 10 ml of the acetone (to maintain a ratio of 1: 50, one part acetone to fift y parts of bleach) into the container. Add some more ice to keep the temperature low. Replacing the cubes that have alr eady melted will ensure this. The bleach must be kept cool as otherwise it will emit fumes of bleach and chloroform. Keep aside for 20 minutes to ensure complete reaction. In a while clouding up ca n be seen with an increase in temperature. Allow time for the reaction to settle. This will take about half an hour, but if after this time also the solution does not appear to be settling, a stir will he lp. Once settled, you will see either be a white powder residue or a bubble at the b ottom. This is chloroform. Pour the solution out with care, ensuring that no powder or bubble leaves the co ntainer. Now the pure chloroform, which remains in the glass container, can be extracted with a separation funnel. Organic Syntheses, Coll. Vol. 6, p.499 (1988); Vol. 52, p.124 (1972). REDUCTIVE AMINATION WITH SODIUM CYANOBOROHYDRIDE: N,N-DIMETHYLCYCLOHEXYLAMINE [Cyclohexanamine, 4,4-dimethyl-] Submitted by Richard F. Borch1 Checked by K. Abe and S. Masamune. 1. Procedure A solution of 21.4 g. (0.262 mole) of dimethylamine hydrochloride in 150 ml. of methanol is prepared in a 500-ml., round-bottomed flask. Potassium hydroxide (4 g.) is added in one portion to the magnetically stirred solution (Note 1). When the pellets are completely dissolved, 19.6 g. (0.200 mole) of cyclohexanone is a dded in one portion. The resulting suspension is stirred at room temperature for 15 minutes before a solution of 4.75 g. (0.0754 mole) of sodium cyanoborohydrid e (Note 2) and (Note 3) in 50 ml. of methanol is added dropwise over 30 minutes to the stirred suspension. After the addition is complete, the suspension is sti rred for 30 minutes. Potassium hydroxide (15 g.) is then added, and stirring is continued until the pellets are completely dissolved. The reaction mixture is fi ltered with suction, and the volume of the filtrate is reduced to approximately 50 ml. with a rotary evaporator while the bath temperature is kept below 45° (Note 4) and (Note 5). To this concentrate is added 10 ml. of water and 25 ml. of sat urated aqueous sodium chloride, and the layers are separated. The aqueous layer is extracted with two 50-ml. portions of diethyl ether. The organic layer previo usly separated and the ethereal extracts are combined and extracted with three 2

Use of material purified by the published procedure2 gives a less colored crude product. Copious amounts of potassium chloride precipitate during this addition. The combined organic layers are washed with 10 ml. 6.4 and by the Leuckart reaction. 3. The composition of this forerun is 80 85% of the amine and 20 15% of th e alcohol. a nd freed of ether with a rotary evaporator (Note 4). GC analysis of the product shows that the product is at least 99. the fraction boiling at 156 159° is collected. 144 155° (Note 11) is separated. of a forerun. GC column packed with 10% Apiezon L and heated to 100°. The submitter reported a 62 69% yield (15. It is normal for additional potassium chloride to precipitate as the evaporat ion continues. Inc. Precipitation of potassium chloride begins immediately.N-Dimethylcyclohexylamine has been prepared by catalytic reductive alkylation3 . 5. b. causing the ether to boil. . 11. should be used for the distill ation.2% pure and is contaminated only with trace amounts of cyclohexanol. n25D 1. as illustrated in Table I.7 17. o f saturated aqueous sodium chloride. This crude product is fract ionated through a 15-cm. and tertiary amines. On a 2-m. and the addition of p otassium hydroxide must be carried out gradually to prevent the contents of the flask from boiling over. portions of 6 M hydrochloric acid (Note 6). r espectively.p. r equires no special apparatus.4521 (Note 12). After 1 3 g.N-dimethylcyclohexylamine.5 The present method is experimentally simple. portions of ether. but makes no improvement in yield or purity of the final product. secondary. portions of ether ( Note 7). the presence of this solid does not interfere with the reaction.5 g. 8.7 g. Since the product boils at 75° (15 mm. 10. 7.N-dimethylcyclohexylamine and cyclohexanol are 15 and 4 minutes. and the aqueous layer is extracted with tw o 40-ml. The initial addition must be carried out with gentle swirling and cooling. Discussion N. 2. 4. Vigreux column (Note 10). care should be exercised to prevent lo ss of material in the evaporation process. and is generally applicable to the synthesis of a variety of primary. 12. A still pot with a volume of at least 100-ml. The layers are separated. (52 54%) of N. dried over anhydrous potassium carbonate. Sodium cyanoborohydride is available as a pale brown solid from Alfa Inorgani cs. since foaming occurs as the distillation proceeds.3 13. The aqueous layer in this step is saturated with ether. GC analysis shows that the ethereal extract contains solely cyclohexanol (>98 %). 3.). 2. Notes 1. the retentio n times for N. The aqueous solution is cooled to 0° in an ice bath and brought to pH > 1 2 by addition of potassium hydroxide pellets to the stirred solution (Note 8) an d (Note 9). yieldin g 13. It is not necessary to remove the salt by filtration before the ether extraction. 9.0-ml. and removal by filtration will resul t in loss of dimethylamine. Caution! This addition of hydrochloric acid into a separatory funnel occurs w ith considerable heat evolution. The combined acid layers are s aturated with sodium chloride and extracted with four 30-ml. The commercially available material can be used without further purification.) using the indicated scale.