反应详情

温度

50 °C

120 g (0.289 mol) racemic 1-(4-benzyloxy-phenyl)-2-(4-hydroxy-4-phenyl-piperidin-1-yl)-1-propanone and 1360 ml acetone were charged to a 3 liter flask equipped with a mechanical stirrer, a thermometer and a reflux condenser. The resulting solution was warmed to 50° C., then 105 g (0.293 mol) di-O-benzoyl-D-tartaric acid was added followed by a 200 ml acetone rinse. The solution was stirred at 50° C. and a suspended solid formed after about 25 minutes. The suspension was stirred as an additional 5 hours at 50° C., and then the mixture was cooled to room temperature over 1 hour. The suspension was filtered and the solid cake was washed with 500 ml acetone. The solid was dried at about 45° C. under vacuum (10 mmHg) overnight, giving 191 g (86% yield) (2S)-1-(4-benzyloxy-phenyl)-2-(4-hydroxy-4-phenyl-piperidin-1-yl)-1-propanone di-O-benzoyl-D-tartaric acid salt.

1. customequipped with a mechanical stirrer
2. washrinse
3. customa suspended solid formed after about 25 minutes
4. stirringThe suspension was stirred as an additional 5 hours at 50° C.
5. temperaturethe mixture was cooled to room temperature over 1 hour
6. filtrationThe suspension was filtered
7. washthe solid cake was washed with 500 ml acetone
8. customThe solid was dried at about 45° C. under vacuum (10 mmHg) overnight