Ammonia → HCID 12234597, compound

Participants

Reaction Steps

To a solution of 50 ml of 1.07 M diborane in tetrahydrofuran was added with stirring 1.43 g of 1-methyl-5-phenyl-7-chloro-1,3-dihydro-2H-1,4-benzodiazepin-2-one at room temperature, and the mixture was refluxed with stirring for 7.5 hours. After having been left standing overnight, 5 ml of water followed by 5 ml concentrated hydrochloric acid was added to decompose the excess diborane, and the mixture was refluxed for one hour. After cooling, the solution was neutralized with concentrated ammonia, and extracted with ether. The ether extract was washed with water and dried over anhydrous sodium sulfate, and the solvent was ramoved under reduced pressure. The residue was recrystallized from n-pentane to obtain 1.30 g of 1-methyl-5-phenyl-7-chloro-2,3,4,5-tetrahydro-1H-1,4-benzodiazepine, melting at 66° to 68° C.

Provenance & Evidence