Chemistry of carbon compounds – Miscellaneous organic carbon compounds – C-metal
Patent
1983-05-25
1984-10-02
Rollins, Alton D.
Chemistry of carbon compounds
Miscellaneous organic carbon compounds
C-metal
2602444, C07D48704
Patent
active
044746997
ABSTRACT:
An improved process for preparing a 1-aminomethyl-6-substituted-4H-s-triazolo[4,3-a][1,4]benzodiazepine product, e.g., adinazolam, directly from the corresponding 1-hydrogen-6-substituted-4H-s-triazolo[4,3-a][1,4]benzodiazepine starting material, e.g., from estazolam, by conducting the reaction between the estazolam-type compound and the dimethylaminomethylene salt in the selected solvent in the presence of an alkali metal carbonate, and thereafter extracting the 1-aminomethyl-6-substituted-4H-s-triazolo[4,3-a]-[1,4]benzodiazepine from an aqueous organic solvent mixture thereof into a halogenated C.sub.1 to C.sub.3 -alkane solvent while maintaining the pH of the aqueous phase between pH 3.0 and 4.0, and thereafter recovering the product from the halogenated alkane solvent.
REFERENCES:
patent: 3987052 (1976-10-01), Hester, Jr.
patent: 4001262 (1977-01-01), Gall
patent: 4250094 (1981-02-01), Hester, Jr.
Hester, J. Org. Chem., vol. 44, pp. 4165-4169, (1979).
Chem. Pharm. Bull., (Japan), 28, (8), 2536-2540, (1980), N. Inotsume, et al., "Reversible . . . Temperature".
Cram Donald J.
Gall Martin
Lipton Michael F.
Reynolds John T.
Rollins Alton D.
The Upjohn Company
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