Water → HCID 54397252, compound

Participants

Reaction Steps

2.5 g (7.5 mmol) of (S)-8-chloro-1-[(Z)-2-chlorovinyl]-11,12,13,13a-tetrahydro-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepin-9-one was heated to boiling under reflux for 5 hours together with 1.66 ml (11.2 mmol) of 1,8-diazabicyclo[5.4.0]undec-7-ene in 30 ml of N,N-dimethylformamide. The reaction mixture was subsequently poured into 400 ml of water and the crystals obtained were filtered off. After drying and recrystallization from N,N-dimethylformamide there was obtained (S)-8-chloro-1-ethynyl-11,12,13,13a-tetrahydro-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepin-9-one of melting point 324°-325°.

Provenance & Evidence