反应详情

温度

100 °C

A solution of [1-(4-trifluoromethyl-phenyl)-piperidin-4-ylmethyl]-carbamic acid tert-butyl ester (45 g; 126 mmol, prepared in accordance with Example 55) in tetrahydrofuran (450 mL) was added over 7 min to a molar solution of lithium aluminium hydride in tetrahydrofuran (377 mL). The resulting mixture was heated to 100° C., and then maintained at that temperature for 195 min. Afterward, the mixture was allowed to cool to room temperature and then poured onto a mixture of ice (500 g) and of 2 N aqueous HCl (350 mL). The organic solvents were removed by evaporation under reduced pressure, and the aqueous phase was basified to a pH of 11 by adding 2 N aqueous NaOH. This resulting in a precipitate, which was filtered and dried at 40° C. under a pressure of 3 mbar to afford the desired product (17.7 g; 65 mmol).

1. temperaturemaintained at that temperature for 195 min
2. temperatureto cool to room temperature
3. customThe organic solvents were removed by evaporation under reduced pressure
4. additionby adding 2 N aqueous NaOH
5. filtrationThis resulting in a precipitate, which was filtered
6. customdried at 40° C. under a pressure of 3 mbar