Potassium Hydroxide → HCID 3054334, compound

Participants

Reaction Conditions

Reaction Steps

15.2 g of the 7-chloro-1-methyl-2-cyanomethylene-5-phenyl-1,3-dihydro-2H-1,4-benzodiazepine obtained in Example 1 A are subsequently portion-wise introduced into 80 ml of concentrated sulfuric acid under stirring, and the resulting suspension is slowly heated up to a temperature of 50° C. until a clear solution is formed. Subsequently, the solution is maintained at a temperature of 50° C. for 1 hour. After cooling, the solution is worked-up by pouring it on ice, neutralizing the sulfuric acid with diluted potassium hydroxide solution and extracting the raw product with methylenechloride. The organic phase is separated, washed with water until neutral reaction of the washing-water, and dried over sodium sulfate. After filtration and evaporation of the solvent a residue is obtained which is re-crystallized from ethanol. 11 g of 7-chloro-1-methyl-2-carbamoylmethylene-5-phenyl-1,3-dihydro-2H-1,4-benzodiazepine, having a melting point of 179° to 181° C., are obtained.

Provenance & Evidence