Novel thiazole route to methamphetamine , Hive Stimulants


		Rhodium (Chief Bee) 10-18-03 09:33 No 465430				Novel thiazole route to methamphetamine (Rated as: good read)
						This is an indeed novel route to methamphetamine... 4-methyl-5-phenyl-thiazole + Sodium Ethoxide -> Methamphetamine Helv.Chim.Acta; 25, 528 (1942) Patent CH233303 Preparations of 4-methyl-5-phenyl-thiazole 1-bromo-1-phenyl-propan-2-one + formamide -> 4-methyl-5-phenyl-thiazole (Benzene, P2S5, 143-147°C/10mmHg, 45%) J.Chem.Soc.Perkin Trans.2, 1538-1543 (1981) 4-methyl-thiazole + Benzoyl Peroxide -> 4-methyl-5-phenyl-thiazole Bull.Soc.Chim.Fr., 3280-3288 (1968) 1-bromo-1-phenyl-propan-2-one + thioformamide -> 4-methyl-5-phenyl-thiazole Helv.Chim.Acta; 25, 528 (1942) 1-chloro-1-phenyl-propan-2-one -> 2,5-dimethyl-3,6-diphenyl-[1,4]dithiane-2,5-diol (Et2O, MeOH, NaHS, H2S, -20°C) 2,5-dimethyl-3,6-diphenyl-[1,4]dithiane-2,5-diol + CH2O + NH3 => 4-methyl-5-phenyl-2,5-dihydro-thiazole 4-methyl-5-phenyl-2,5-dihydro-thiazole + Sulfur -> 4-methyl-5-phenyl-thiazole Justus Liebigs Ann. Chem.; 615, 77, 83 (1958) Bull.Soc.Chim.Fr. 4514 (1967) Bull.Soc.Chim.Fr. 4521 (1967) C.R.Hebd.Seances Acad.Sci.Ser.C 262, 687 (1966) C.R.Hebd.Seances Acad.Sci.Ser.C 264, 336 (1967) C.R.Hebd.Seances Acad.Sci.Ser.C 265, 744 (1967) C.R.Hebd.Seances Acad.Sci.Ser.C 266, 822 (1968)



		RepVip (Hive Bee) 10-20-03 11:21 No 465796				Articles
						What are the chances of getting a copy of these articles in english: Helv.Chim.Acta; 25, 528 (1942) Bull.Soc.Chim.Fr., 3280-3288 (1968) ? EDIT: Actually, if it's possible just to get a copy of Bull.Soc.Chim.Fr., 3280-3288 (1968) I may know someone who can translate it--though I'm sure she'd be suspicious



		Rhodium (Chief Bee) 11-25-03 01:00 No 473042				Methamphetamine via 2-Methylisoxazolin-5-one (Rated as: excellent)
						I have never before seen such a well-hidden synthesis of methamphetamine in an article before - it is really hard to spot that they are actually synthesizing it from one of their isoxazolines (check the article yourself). 2-Methylisoxazolin-5-ones. Part I. F. DeSarlo, L. Fabbrini, G. Renzi Tetrahedron 22, 2989-2994 (1966) (../rhodium/pdf /meth.2-methylisoxazolin-5-one.pdf) 2,3-Dimethyl-4-phenylisoxazolin-5-one (IX) Ethyl alpha-phenylacetoacetate (0.1 mole) and N-methylhydroxylamine hydrochloride (0.45 mole) in anhydrous pyridine (100 ml) were heated at 100°C for 12 hr. The residue after evaporation of the solvent was washed with ether, then with water, yield 91%; mp 112-113°C (ligroin). In alcohol, as reaction solvent, the yield was 73%. Hydrogenation of IX A solution of IX (0.02 moles) in 150 ml anhydrous EtOH^* was shaken for 1 day under a 3-4 atm. H₂ pressure, with Raney Ni. After the absorption of 0.04 moles H₂, the solution was filtered and fractionated to isolate N-Methylamphetamine (XIV); bp 38°C/0.3 torr; 208°C/750 torr. mp of the hydrochloride 129-134°C. * If 95% EtOH was used instead of anhydrous, the compound only absorbed 1 equivalent of H₂ and the product was instead the intermediate imine. Precursor Synthesis *Ethyl Phenylacetate + Ethyl Acetate -> Ethyl alpha-Phenylacetoacetate* J. Amer. Chem. Soc. 69, 119 (1947) J. Chem. Soc. 123, 1764 (1923) Chem. Ber. 63, 1557 (1930) Chem. Ber. 66, 1512 (1933) Phenylacetonitrile + Ethyl Acetate -> Phenylacetoacetonitrile Organic Syntheses, Coll. Vol. 2, p. 487 (http://www.orgsyn.org/orgsyn/prep.asp?prep=cv2p0487) *Phenylacetoacetonitrile -> Ethyl alpha-Phenylacetoacetate* Organic Syntheses, Coll. Vol. 2, p. 284 (http://www.orgsyn.org/orgsyn/prep.asp?prep=cv2p0284)



		psilocin (Stranger) 11-25-03 01:35 No 473046				wow
						nice! other hydrogenation possibilities?



		Rhodium (Chief Bee) 11-25-03 02:18 No 473049				That's left as an exercise for the reader
						That is very likely, but it is not in the literature as the 5-isoxazolinone is a pretty uncommon ring system.



		WizardX (Wizard Master) 11-25-03 19:34 No 473224				Also...
						Also... P2P from a-Phenylacetoacetonitrile http://www.orgsyn.org/orgsyn/prep.asp?prep=cv2p0389 This is why benzyl cyanide and phenyl acetic acid is so HIGHLY RESTRICTED.



		Rhodium (Chief Bee) 03-17-04 12:50 No 495784				5-Phenyl-4-Methyl-Thiazole to Methamphetamine (Rated as: good read)
						^{Reference from Post 465430 (Rhodium: "Novel thiazole route to methamphetamine", Stimulants)} _{Strukturchemishe Untersuchungen IV.} Über eine reduzierende Aufspaltung des 5-Phenyl-4-methyl-thiazols H. P. Schenk and D. Lamparsky Journal of Chromatography, 204, 391-395 (1981) (../rhodium/pdf /nutmeg.oil.analysis.pdf) Summary: Sodium metal reduction of 5-Phenyl-4-Methyl-Thiazole to Methamphetamine. ^{The Hive - Clandestine Chemists Without Borders}