Ammonium Hydroxide → HCID 69021420, compound

Participants

Reaction Conditions

Reaction Steps

NaBH3CN (0.0472 mol) was added at 5° C. to a mixture of intermediate (7) (0.0236 mol) in acetic acid (50 ml) and methanol (300 ml). The mixture was stirred at 5° C. for 30 min and then stirred at room temperature for 2 hours. Ice water and then NH4OH 35% (60 ml) were added. The mixture was stirred for 2 hours. The precipitate was filtered off, washed with water and taken up in DCM. The organic layer was separated, dried (MgSO4), filtered and the solvent was evaporated, yielding 8.25 g (85%) of 7-(4-chlorobenzoyl)-5-(3-chlorophenyl)-1,3,4,5-tetrahydro-1-methyl-2H-1,4-benzodiazepin-2-one (intermediate 8), mp. 177° C.

Provenance & Evidence