反应详情

温度

0 °C

To an ice-cold solution of 286.4 g (0.914 mole) of 4-hydroxy-(4-toluenesulfonyl)-D-proline ethyl ester (5) in 2.8 L of tetrahydrofuran was added 20 g (0.918 mole) of lithium borohydride in one portion. The mixture was stirred at 0° C. for 1 hour and then kept at a temperature below 25° C. overnight. The mixture was cooled to 0° C. and the pH adjusted to 3 with 6N hydrochloric acid (180 ml). The volume was reduced to 500 ml by rotary evaporation, and 1.5 L of water was added. The white precipitate was filtered, washed with cold water (500 ml) dried under reduce pressure to give 223.8 g (90%) of the title compound. M.P.=127° C.

1. customkept at a temperature below 25° C. overnight
2. temperatureThe mixture was cooled to 0° C.
3. customThe volume was reduced to 500 ml by rotary evaporation, and 1.5 L of water
4. additionwas added
5. filtrationThe white precipitate was filtered
6. washwashed with cold water (500 ml)
7. customdried