4,5-Dihydrodiazepam → HCID 21414257, compound

Participants

Reaction Steps

1 g. of 1-methyl-5-phenyl-7-chloro-1,3,4,5-tetrahydro-2H-1,4-benzodiazepine-2-one and 1 g. of magnesium oxide are added to a solution of 0.8 g. (2.29 mmoles) of 1-methyl-4-chlorocarbonyl-5-phenyl-7-chloro-1,3,4,5-tetrahydro-2H-1,4-benzodiazepine-2-one in 10 ml. of chloroform, and the mixture is stirred at 40° C. overnight. Thereafter the inorganic salts are filtered off, washed with 10 ml. of chloroform, and the chloroform solution is stirred with 10 ml. of 2n hydrochloric acid. The hydrochloride of the non-reacted base separates. The salt is filtered off, and the filtrate is washed with 5 ml. of 2.5 % aqueous sodium hydrocarbonate solution and with water. The chloroform solution is dried and evaporated. The obtained dry residue is recrystallized from ethanol. 0.91 g. (66.2 %) of di-(1-methyl-2-oxo-5-phenyl-7-chloro-1,3,4,5-tetrahydro-2H-1,4-benzodiazepine-4-yl)-ketone are obtained; m.p.: 263°-266° C., Rf2 = 0.71.

Provenance & Evidence