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ChemicalBook CAS DataBase List N-desalkylflurazepam

N-desalkylflurazepam synthesis

12synthesis methods
-

Yield:2886-65-9 71%

Reaction Conditions:

with paraformaldehyde in methanol;ammonia;water;

Steps:

18 EXAMPLE 18

EXAMPLE 18 Paraformaldehyde (147.2 g., 91% flake) is placed in a stirred reactor equipped with an ammonia addition tube and a reflux condenser. Methanol (550 mls.) is added, along with 2-chloroacetamido-5-chloro-2'-fluorobenzophenone (326.2 g.) at room temperature. The reaction mixture is stirred and ammonia gas bubbled in below the surface of the reaction mixture. The reaction mixture was then heated at reflux for 10 hours with a steady flow of ammonia gas. Cool to room temperature and filter the crystalline product obtained. Wash product with cold methanol (2 * 125 mls. at -10° C.), followed by hot water (4 * 500 mls at 60° C.). When dry, there was obtained 7-chloro-1,3-dihydro-5-(2-fluorophenyl)-2H-1,4-benzodiazepin-2-one (205 g., 71%) m.p. 205.5°-207° C. (uncorr.).

References:

US3996209,1976,A

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