反应详情

To the reaction mixture of Example 6 was added sodium borohydride (0.1 m=3.9 g) along with some water (8.7 mL). After stirring at room temperature for 3 hours, the reaction mixture was slowly added to excess amount of water (540 ml) with stirring. The wet filter cake was washed with 270 mL of water, then crystallized from 355 g of butyl chloride to give a crude product. Recrystallization from 300 g of ethyl acetate and dried in a vacuum oven to give 49.3 g of pure title compound in 72% yield for two steps, mp 168°-169° C.

1. stirringwith stirring
2. washThe wet filter cake was washed with 270 mL of water
3. customcrystallized from 355 g of butyl chloride
4. customto give a crude product
5. customRecrystallization from 300 g of ethyl acetate
6. customdried in a vacuum oven