Pyridine → HCID 20393037, compound

Participants

Reaction Conditions

Reaction Steps

50 ml of a 20% solution of phosgene in toluene were added dropwise over a period of 10 minutes to a mixture consisting of 10.0 gm of 6,11-dihydro-2,4,6-trimethyl-5H-pyrido[2,3-b][1,5]-benzodiazepin-5-one, 100 ml of diethyl ketone, 50 ml of toluene and 5 ml of pyridine. The resulting mixture was heated at 60° C. for 2 hours, at 80° C. for one hour and at 110° C. for one hour, while stirring. After cooling to room temperature, 100 ml of water were added. The organic phase was dried with sodium sulfate and then evaporated in vacuo. The residue was recrystallized twice from ethanol, yielding 7.3 gm of 11-chloroformyl-6,11-dihydro-2,4,6-trimethyl-5H-pyrido[2,3-b][1,5]benzodiazepin-5-one, m.p. 205°-207° C.

Provenance & Evidence