反应详情

温度

50 °C

A solution of 100 mg (0.27 mmol) of ((S)-5-methanesulfonyl-1-methyl-2-oxo-2,3,4,5-tetrahydro-1H-benzo[b][1,4]diazepin-3-yl)-carbamic acid tert-butyl ester in 5 ml of dioxane was treated with 0.22 ml of hydrochloric acid and heated in the sealed flask at 50° C. for 1 hour. For the working-up, the solvent was evaporated under reduced pressure and the residue submitted to a azeotropic distillation with toluene. After drying under reduced pressure, the (S)-3-amino-5-methanesulfonyl-1-methyl-1,3,4,5-tetrahydro-benzo[b][1,4]diazepin-2-one hydrochloride was obtained in quantitative yield as a light yellow solid; MS: m/e=270 (M+H)+.

1. customthe solvent was evaporated under reduced pressure
2. distillationthe residue submitted to a azeotropic distillation with toluene
3. customAfter drying under reduced pressure