反应详情

To a solution of ester 138 (2.65 g, 6.14 mmol) in 20 mL THF at 0° C. was added a precooled (0° C.) solution of LiOH monohydrate (1.0 g, 23.8 mmol) and hydrogen peroxide (30 wt % aqueous soln, 5.0 mL) in 10 mL H2O. The mixture was stirred vigorously for 90 minutes, then warmed to ambient temperature and stirred 90 minutes. The reaction was quenched at 0° C. by addition of 100 mL 10% NaHSO3 (aq), then extracted with Et2O. The phases were separated, and the organic phase washed with brine, dried (MgSO4), and concentrated. The crude acid 139 was used without purification.

1. stirringstirred 90 minutes
2. customThe reaction was quenched at 0° C. by addition of 100 mL 10% NaHSO3 (aq)
3. extractionextracted with Et2O
4. customThe phases were separated
5. washthe organic phase washed with brine
6. dry with materialdried (MgSO4)
7. concentrationconcentrated
8. customThe crude acid 139 was used without purification