Sodium Hydroxide → HCID 70042193, compound

Participants

Reaction Steps

4 g (10.83 mmol) of t-butyl (S)-11,12,13,13a-tetrahydro-8-methylthio-9-oxo-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepine-1-carboxylate are dissolved in 50 ml of methylene chloride and treated portionwise at room temperature with 4.0 g (about 20.8 mmol) of about 90 percent m-chloroperbenzoic acid. Subsequently, the mixture is warmed to boiling under reflux for 2.5 hours, then poured into 2 N sodium hydroxide and the methylene chloride solution is separated. The organic phase is dried over magnesium sulphate and evaporated. After recrystallization from chloroform/hexane, there is obtained t-butyl (S)-11,12,13,13a-tetrahydro-8-methylsulphonyl-9-oxo-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepine-1-carboxylate of melting point 244°.

Provenance & Evidence