反应详情

To a solution of [4-(1,3,3-trimethyl-6-aza-bicyclo[3.2.1]octane-6-carbonyl)-phenyl]carbamic acid tert-butyl ester (11.78 g, 31.61 mmol) in DCM (150 ml) was added TFA (50 ml). The resulting mixture was stirred for 48 hrs. at room temperature and evaporated in vacuo. To the residue was added water (150 ml) and diethyl ether (50 ml) and the pH was adjusted to 8 by addition of 32% aq. sodium hydroxide. The mixture was stirred for 15 min., the precipitate filtered off, washed with water and dried in vacuo at 50° C. for 18 hrs. affording 8.4 g (98%) of the title compound as a solid.

1. customat room temperature and evaporated in vacuo
2. additionTo the residue was added water (150 ml) and diethyl ether (50 ml)
3. additionthe pH was adjusted to 8 by addition of 32% aq. sodium hydroxide
4. stirringThe mixture was stirred for 15 min.
5. filtrationthe precipitate filtered off
6. washwashed with water
7. customdried in vacuo at 50° C. for 18 hrs