Ammonia → HCID 12317899, compound

Participants

Reaction Steps

A mixture of 3.6 g. (0.01 mol) of 5-(2-chlorophenyl)-1,3-dihydro-1-methoxymethyl-7-nitro-2H-1,4-benzodiazepin-2-one, 100 ml. of tetrahydrofuran, 50 ml. of methanol, 13.6 g. of sodium acetate trihydrate and 11.25 g. of stannous chloride dihydrate was stirred under nitrogen for 5 hours. 500 ml. of methylene chloride and 10 ml. of concentrated ammonia was added. The inorganic material was separated by filtration. The filtrate was washed with 1N sodium hydroxide solution, dried over sodium sulfate and evaporated. Crystallization of the residue from methylene chloride/ether gave light yellow product with m.p. 205°-208° dec. For analysis it was recrystallized from 2 -propanol/tetrahydrofuran.

Provenance & Evidence