Dichloromethane → HCID 20516784, compound

Participants

Reaction Steps

A solution of 50 g (0.175 mol) of 7-amino-5-(o-fluorophenyl)-1,3-dihydro-1-methyl-2H-1,4-benzodiazepin-2-one in 700 ml of methylene chloride is treated at room temperature with 27 g of N-chlorosuccinimide and the mixture is stirred for 1 hour. Subsequently, a further 27 g of N-chlorosuccinimide are added and the mixture obtained is stirred at room temperature for 17 hours. The mixture is diluted with methylene chloride, the organic phase is washed with 2 N sodium carbonate solution, dried and evaporated. After chromatography on 200 g of silica gel using methylene chloride for the elution, the residue gives 7-amino-6,8-dichloro-5-(o-fluorophenyl)-1,3-dihydro-1-methyl-2H-1,4-benzodiazepin-2-one which melts at 234° C. after recrystallisation from methylene chloride/ethyl acetate.

Provenance & Evidence