反应详情

Compound 61 (32.1 g, 0.11 mol) is mixed with LiOH (10% in water, 50 mL), THF (100 mL), MeOH (30 mL) and a catalytic amount (˜20 mg) tetrabutylammonium iodide in a 500 mL flask. This mixture is heated at reflux overnight, allowed to cool to room temperature, and acidified with concentrated HCl. The resultant yellow solid is collected by filtration and washed thoroughly with water. The solid then is heated with hexane (100 mL) allowed to cool to room temperature. After filtration, the solid is collected, dried over vacuum to yield compound 62 as a light yellow powder (28.0 g, 96.7% yield). M.P.: 110.7-112.4° C.

1. temperatureThis mixture is heated
2. temperatureat reflux overnight
3. filtrationThe resultant yellow solid is collected by filtration
4. washwashed thoroughly with water
5. temperatureThe solid then is heated with hexane (100 mL)
6. temperatureto cool to room temperature
7. filtrationAfter filtration
8. customthe solid is collected
9. customdried over vacuum