反应详情

To a stirred solution of 66.32A (1.00 g, 3.5 mmol) in THF (70.0 mL) and MeOH (70.0 mL) at 0° C. was slowly added potassium hydroxide (1.9 mL, 3.8 mmol) to maintain the temperature below 6° C. The reaction mixture was allowed to warm to room temperature and stirred for 48 hours. The reaction mixture was then concentrated in vacuo, acidified with 1N HCl, and extracted three times with EtOAc. After drying over anhydrous magnesium sulfate and filtering, the organic solvent was removed under reduced pressure and to give a white solid 66.32B (0.90 g, 95% yield).

1. customat 0° C.
2. temperatureto maintain the temperature below 6° C
3. concentrationThe reaction mixture was then concentrated in vacuo
4. extractionextracted three times with EtOAc
5. dry with materialAfter drying over anhydrous magnesium sulfate
6. filtrationfiltering
7. customthe organic solvent was removed under reduced pressure