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INTRODUCTION The most common method of manufacture of methamphetamine in the United States is the reduction of e with hydriodic acid and red phosphorus (HI/red P)1.html 5/7/2004 . mechanism. It greater than 95% in purity and contains no ephedrine.rhodium. whereas the reduction of (-)-ephedrine pseudoephedrine yields (+)-methamphetamine. red phosphorus. the latter being converted to phosph phosphoric acids7. The salt is filtered and dr theoretical yield is 92% by weight of the precursor ephedrine. made basic. Emde incorrectly cites Ogata6 as produc methamphetamine in 1919 by heating (-)-ephedrine or (+)-pseudoephedrine with HI and yellow phospho clandestine manufacture of (+)-methamphetamine from (-)-ephedrine or (+)-pseudoephedrine is a ver process. hali alcohols2. and hydriodic acid is heated. 48 128-134 (1990) HTML by Rhodium SUMMARY The illicit manufacture of methamphetamine from ephedrine via reduction with hydriodic acid and rod phosphorus is discussed. A mixture of ephedrine.Methamphetamine Synthesis Via HI/Red Phosphorous Reduction of Ephedrine .rh. Even though the HI/red P ephedrine reduction method is relatively new (1982) in clandestine laborato method has been known for many years and has been used to reduce carbonyl groups. "Freon-11') and hydrogen chloride gas. RESULTS AND DISCUSSION The HI/red P reduction of ephedrine to methamphetamine involves a cyclic oxidation of the iodide anion and reduction of iodine back to the anion by the red phosphorus. The stereochemistry.ws/chemistry/meth.. nitrites.[www. The stereospecificity of the reduction results from mechanistic factors as well as the diastereoisomeric natu http://www. SKINNER FORENSIC SCIENCE INTERNATIONAL..and bromoephedrines by Emde4 and Schmidt5 usin reduction methods not including the HI/red P method.rhodium.3.ws] [] [Chemistry Archive]     Search METHAMPHETAMINE SYNTHESIS VIA HI/RED PHOSPHOROUS REDUCTION OF EPHEDRINE HARRY F. Reduction of ephedrine to methamphetamine is well documented in the literature. The final product varies from white to orange/brown in color. extra crystallized as the hydrochloride salt from ether/acetone with hydrochloric acid or hydrogen chloride gas trichloromonofluoromethane (i. synthetic impurities. Page 1 of 3 [www. The configu ephedrine were determined by reduction of the chloro.hi-rp.8. filtered.e. Manufacture of methamphetamine from phenyl-2-p (P2P) and methylamine yields (±)-methamphetamine. whereas the clandestine yields range from 5 by weight of the precursor ephedrine. and analysis of clandestine methamphetamine samples are addressed.

methamphetamine HCl can be separated by washing the solid with chloroform. wh enantiomers reduce to (-)-methamphetamine.hi-rp. The interesting aspect of the HI/red P ephedrine reduction is that P2P is produced as an impurity in the s Normally.Methamphetamine Synthesis Via HI/Red Phosphorous Reduction of Ephedrine . single and multiple phase liquids w range of 1-14. The valuable property of the HI ion-pair is that methamp HI can be extracted from an aqueous solution with chloroform. 2 carbons of the propane chain.ephedrine HCl.12. In cas ephedrine HCl is present. First. If the HI/red P reaction is incomplete. Ephedrine once exposed to hydriodic acid can form an ion-pair with the hydriodide.ws/chemistry/meth. Partial conversion will obviou in a mixture of the HI salts being obtained. The methamphetamin in the reaction also can form an ion pair with the hydriodide. can be easily identifi GC/MS can also be used to identify methamphetamine.rhodium. The (±) mixture of either ephedrine reduces to methamphetamine.methamphetamine HCl. the IR spectrum of the (±)-mixture differs from the enantiomers.and trans-1. 1 carbon. (-)-ephedrine and (+)-pseudoephedrine. The chloroform extract is evaporated and the light yellow cr methamphetamine HI are identified by IR. The 'aziridines' can undergo a ring opening acidic hydrolysis to form p propanone. solids. The HCl and HI salts of methamphetamine insoluble in ether and soluble in chloroform and very soluble in water.2-dim phenylaziridine. an ether wash is required to remove the neutral P2P and 'naphthalene' impur is followed by a chloroform extraction. The 'aziridines' (cis. 1. Methamphetamine. The chloroform portion .). The enantiomer and diastereoisomer of ephedrine selected as the precursor dicta isomer of methamphetamine will be produced. ANALYSIS Samples from HI/red P laboratories vary from bottled precursors.. The P2P forms an aldol condensation product with subsequent dehydration to form the 'nap impurities. discovery of P2P in a clandestine laboratory indicates that (±)-methamphetamine. either from addition as an adulterant or from incomplete conversion of the ephedrine. The enantiomeric (+) and (-) s identical IR spectra. to sludges. However. Page 2 of 3 ephedrines.rh. and pesudoephedrine HI salts yellow solids at room temperature. f from iodoephedrine is more likely. The diastereoisomers. The 'aziridines' can be reduced to methamphetamine or react to impurities found in the reaction. pers. This method of identification will also wor discarded red P sludge. The HI salts of the ephedrines also have similar properties. Methamphetamine HCl will not ext chloroform from an aqueous solution. 1 and No. Ephedri with HI to form iodoephedrine (iodomethamphetamine) which is predominately reduced to methamph Iodoephedrine can undergo a ring closure to form 'aziridines'. since the enantiomer of the methamphetamine product depends solely on the enantiom ephedrine precursor. Identification of methamphetamine is easily made by direct infrared analys finished product or acid/base extraction of most samples with subsequent conversion to the HCl salt.html 5/7/2004 . ephedrine. is the However. However.[www.. W. Methamp HI can be identified by IR from the original reaction mixture.. comm. and the chloroform soluble portion . Ephedrine and pseudoephedrine are 1-phenyl-1-hydroxy-2-methylamino-propane. The transient existence of iodoephedrine was indirectly by the total 'aziridines'. each cont chiral centers at the No.3-dimethyl-2-phenylnaphthalene and 1-benzyl-3-methylnaphthalene10. ephedrine HI or pseudoephedrine HI can be identified by their IR using the same extraction procedures given above for methamphetamine HI. The non-acidic red chloroephedrine produces the 'aziridines' but no P2P11. Reduction to methamphetamine elimi chiral center at the No. the P2P is formed as an impurity and has no bearing on the enantiomeric form of the sy methamphetamine. are reduced to (+)-methamphetamine. The HI salt is readily soluble in unlike the HCl salt which is only slightly soluble. http://www. The reaction mechanism for the reduction of ephedrine with HI/red P is summarized as follows. Racemic methamphetamine HI is an oil. The analogous chloroephedrines undergo thermal decomposition to the 'a in the injection port of the gas chromatograph (Martin. The neutral P2P and 'naphthalene' impurities can be extracted from the methamphetamine in the origina mixture (acidic with HI) or any other acidic solution in the clandestine laboratory and can be identified GC/MS techniques. mol wt 147) could also be formed directly from ephedrine by acid dehydration9.

html 5/7/2004 . a secondary amine. 252. Durrant. Quantitation of both solid and liquid samples found in HI/red P laboratories is routinely done by HPLC and retention times of compounds are given in Table 1. Chim.Methamphetamine Synthesis Via HI/Red Phosphorous Reduction of Ephedrine . 4. Helv. Acta.O. impurities. Page 3 of 3 Identification of (+)-methamphetamine HI indicates that either (-)-Ephedrine or (+)-pseudoephedrine was via the hydriodic acid/red phosphorus method. mixed microcrystals. The blue color is formed imm after the second part of the reagent is added. Emde. L.rh. and products. Chem. Wiley and Sons. 29. The nitroprusside (sodium nitroprusside) reagent reacts to give a deep blue color with secondary amines no color change with primary and tertiary amines. 11. a highly poisonous gas. Int. Abstracts 14. Rinser. 332. A. L. H. 9. Wiley and Sons. Analysis of an HI/red P clandestine laboratory in the field presents hazards.rhodium. also liberate iodine with sulfuric acid. 1922. Vol. T. Pearson. Red phosphorus is a flammable/explosive solid and must be handled w Phosphine. Pharm. Jobuson and A. Ephedrine. 2. 710. 400 (1983). T. deep blue color) from amphetamine and dimethylamphetamine (prim tertiary amines. Fieser. 1989. 32. gives a faint blue c first part of the reagent is prepared by mixing 25 ml of a one percent sodium nitroprusside solution w acetaldehyde. Reagents for Organic Synthesis. Angew Chem. HI is a toxic and strong irr contact must be minimized. no color). 12. 745 (1920) S. John. mixed melting points. CONCLUSION The hydriodic acid/red phosphorus reduction of ephedrine to methamphetamine has been discus stereochemistry of the reaction has been shown as well as the route of reaction to the impurities and produ obtained from IR spectroscopy and GC/MS spectroscopy have been presented to aid in the analys precursors. The dark brown color is caused by t formed from the reaction of sulfuric acid with iodide ion. Schmidt.hi-rp. N. 7 and p. P. intermediates. Pharm. in enantiomeric derivatization GC techniques. all of the methamphetamine and ephedrine hydriodides. 1. 180174z (1984) 13. Jpn.C. Chem. 1962. Methamphetamine from Ephedrine: 1. http://www. 171. Arch.ws/chemistry/meth. Allen and W. Introduction to Advanced Inorganic Chemistry.. Soc. 451. 67. Most organic iodides also produce the same reac sulfuric acid. p. A study of impurities found in methamphetamine syn from ephedrine. Menor. 39. 8. 365 (1929) E. can be produced by careless heating of the HI/red P mixture.. the Marquis reagent is not a useful test for methamphetamine HI. Auterhuff. Identification of P2P and the 'naphthalenes' as impur indicates an ephedrine was reduced under acidic conditions. The enantiomeric form of methamphetamine or ephe determined by one or more of the following: polarimetry. J.S. p. 5. Comprehensive Treatise on Inorg. Allen.. Chem. The nitroprusside13 screening reagent can be used to diff methamphetamine (secondary amine. 89 (1914) E. Buehler and D. Statistical Reports. The normal screening test for amphetamines is the Marquis reagent which turns orange to orange/brown. 1970. REFERENCES Drug Enforcement Administration. and Theor. 39-53 (1988) 11. For example. Wiley. 6. Rishi.. The second part is a two percent sodium carbonate solution.. Survey of Organic Synthesis. Fieser and M. Abstracts. Cantrell. Chloroephedrines and Aziridines. J. 4826c. Abstracts. 3. p. Sci. Vol. Eisei Kayaku. p. Forensic Sci. 100. Chem.[www. 1. Longsman. C. 10.C. 426 (1955). as well as sodium and p iodide. 50. 751 (1919). 7. Ogata. 953-982 (1987) 12. 1967. Methamphetamine HI reacts with the re give an immediate dark brown color with the evolution of iodine. B. 449.

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