反应详情

温度

70 °C

Paraformaldehyde (0.15 g, 0.5 mmol) was added in one portion to pressure vessel containing [1-(4-amino-benzenesulfonyl)-piperidin-4-yl]-carbamic acid tert-butyl ester (0.12 g, 0.34 mmol) in Methanol (5 ml) at room temperature. To this mixture was added sodium methoxide (0.055 g, 1.02 mmol) in one portion, the pressure vessel was sealed and heated at 70° C. for 12 hours. After this time the reaction was cooled to room temperature and sodium borohydride (0.031 g, 0.82 mmol) added in one portion, the pressure vessel was re-sealed and heated at 70° C. for 1 hour. The reaction was then cooled to room temperature, diluted with DCM (20 ml) and washed with water (20 ml). The organic layer was separated, dried (MgSO4), filtered and concentrated to give the title compound (0.13 g, 99% yield) as a white solid which was taken on without further purification. Tr=1.96 min m/z (ES+) (M+Na+) 392.

1. customthe pressure vessel was sealed
2. temperatureAfter this time the reaction was cooled to room temperature
3. customthe pressure vessel was re-sealed
4. temperatureheated at 70° C. for 1 hour
5. temperatureThe reaction was then cooled to room temperature
6. washwashed with water (20 ml)
7. customThe organic layer was separated
8. dry with materialdried (MgSO4)
9. filtrationfiltered
10. concentrationconcentrated