反应详情

A solution of the product from Example 5 (1 g, 3.24 mmol) and benzaldehyde (0.71 mL, 7 mmol) in 2:1 MeOH/H2O (50 mL) was treated with sodium cyanoborohydride (0.56 g, 9 mmol) portionwise under nitrogen and stirred for six hours. The reaction mixture was then added to dichloromethane (150 mL) and washed with saturated sodium bicarbonate. The organic layer was dried over magnesium sulfate and activated charcoal, filtered through a plug of silica gel and concentrated under vacuum to dryness. The solids were triturated in hexane, filtered, and oven dried to give the title compound (0.73 g, 62% yield) as an orange solid, mp=150-152° C.

1. washwashed with saturated sodium bicarbonate
2. dry with materialThe organic layer was dried over magnesium sulfate and activated charcoal
3. filtrationfiltered through a plug of silica gel
4. concentrationconcentrated under vacuum to dryness
5. customThe solids were triturated in hexane
6. filtrationfiltered
7. customoven dried