反应详情

温度

117.5 °C

A 0.2 l reactor was loaded with 70% sulfuric acid (200 g) containing compound 26 (10 g, 0.031 mole), and was heated to 115-120° C. for 5-10 hours, and then cooled to room temperature, i.e., about 20° to about 25° C. An aqueous 40% sodium hydroxide solution was added in an amount sufficient to provide a pH of 1. The solution was then extracted with 35 ml of iso-butanol, the organic layer was separated, and Bu3N was added in an amount sufficient to provide a pH of 4. The (S)-Pregabalin was precipitated, filtered, and washed with 10 ml of iso-butanol. After drying at 55° C. under vacuum, (S)-Pregabalin was obtained as white crystals in a 40.4% yield. Purity: 99.95% area by HPLC.

1. temperaturecooled to room temperature
2. customi.e., about 20° to about 25° C
3. customto provide a pH of 1
4. extractionThe solution was then extracted with 35 ml of iso-butanol
5. customthe organic layer was separated
6. additionBu3N was added in an amount sufficient
7. customto provide a pH of 4
8. customThe (S)-Pregabalin was precipitated
9. filtrationfiltered
10. washwashed with 10 ml of iso-butanol
11. customAfter drying at 55° C. under vacuum