murmur
(HyperLab Bee) 06-02-03 11:13 No 437170 |
Some more reference | Bookmark | ||||||
Journal of Chemical Research (S) 1981, 192 Dibenzo-18-crown-6 as phase transfer catalyst in Bockmuhl's synthesis of methadone http://hyperlab.bravepages.com/JChemRes1 I could't get the Miniprit version of this artcle because in a library this volume is not available. |
||||||||
Rhodium (Chief Bee) 06-02-03 16:18 No 437232 |
Miniprint | Bookmark | ||||||
Edit: The full Miniprint edition has been posted in Post 481630 (Aurelius: "PTC Synthesis of Methadone", Methods Discourse) |
||||||||
murmur (HyperLab Bee) 06-04-03 12:32 No 437755 |
Deuterated Methadone (Rated as: excellent) |
Bookmark | ||||||
Synthesis and Physico-Chemical Properties of (RS)-6-bis(Trideuteriomethyl)amino-4,4-Diphenylhep B.M. Gérardy, et. al. J. Lab. Comp. Radiopharm. 22(1), 5-22 (1985) (../rhodium/djvu /methadone-d Experimental section (R,S)-2,2-diphenyl-4-ditrideuteromethyla To a solution of 6 g (68.5 mmol) of ditrideuteromethylamine hydrochloride dissolved in 3 ml of water was added 2.8 g (70 mmol) of NaOH disolved in 5 ml H2O. Under stirring, a filtered solution of the above mixture was added over 1 h period to 4.77 g (82.2 mmol) of freshly redistilled propylene oxide. After 12 hrs at RT, 90 ml of benzene were added and the reaction mixture was fractionnally distilled. The fractions under 81 °C and above 99°C were discarded. The remaining 4.07 g consisting of a mixture of isomeric aminoalcohols (1-ditrideutromethylamino-2-propanol and 2-ditrideutromethylamino-1-propanol)were (R,S)-4,4-diphenyl-6-ditrideuteromethyla This material was synthesed according to the procedure described by Bockmuhl and Ehrhardt (J.Liebigs Ann.Chem 561(1949)52, Post 483448 (Rhodium: "Bockmühl's Original Methadone Synthesis", Methods Discourse)). To a suspension of 0.24 g (10 mmol) of Mg in 5 ml of dry ether was added 2.55 g (23 mmol) of ethyl bromide. After of completition of the reaction, a solution of 2.8 g (9.86 mmol) of(1) in 3 ml of dry xylene was added to the reaction mixture under stirring. The ether was distilled off in dry conditions; the reaction mixture was heated under reflux for 1 h and then decomposed with 100 ml of 8 N HCl. After the usual work up, 2.48 g (79%) of (2) were obtained. The hydrochloride crystallized from ethanolic HCl was obtained in 72% yield. It was recrystallized from IPA to constant melting point (mp=233°C) This product was pure in GLC and HPTLC. |
||||||||
murmur (HyperLab Bee) 06-09-03 11:19 No 438801 |
Tritiated Methadone (Rated as: good read) |
Bookmark | ||||||
Preparation of Methadone and Some Congeners Labeled with Tritium in the Aromatic Rings J.A. Kepler, et. al. J. Lab. Comp. Radiopharm. 19(2), 271-282 (1982) (../rhodium/djvu /methadone-t |
||||||||