反应详情

温度

23 °C

Lithium borohydride (435 mg, 20 mmol) was added to a solution of ester 3 (2.3 g, 10 mmol) in Et2O (20 mL) at 0° C. After having stirred for 5 min, MeOH (640 mg, 20 mmol) was added dropwise and stirring continued at 0° C. until effervescence ceased. The mixture was warmed to 23° C. and was allowed to stir an additional hour, at which time the mixture was poured into 3N NaOH and stirred an additional 0.5 h. The organic layer was separated and washed with brine, dried (Na2SO4), filtered and concentrated in vacuo. The crude alcohol 4 was purified by FCC (silica gel, 1:1, hexane/CH2Cl2).

1. stirringstirring
2. customcontinued at 0° C. until effervescence
3. stirringto stir an additional hour, at which time the mixture
4. stirringstirred an additional 0.5 h
5. customThe organic layer was separated
6. washwashed with brine
7. dry with materialdried (Na2SO4)
8. filtrationfiltered
9. concentrationconcentrated in vacuo
10. customThe crude alcohol 4 was purified by FCC (silica gel, 1:1, hexane/CH2Cl2)