反应详情

To the stirred solution of compound 8 (0.85 g, 2.45 mmol) in dry THF was added (Cy)2BH (0.87 g, 4.91 mmol) slowly at 0° C. under argon atmosphere. The reaction mixture was warmed to room temperature and stirred for 12 h. The reaction mixture was quenched with 2N NaOH (6 mL) and H2O2 (3 mL) at 0° C. and allowed to stir for 4 h. Then crude reaction mixture was extracted with ethyl acetate (40 mL), washed with water (10 mL), brine (10 mL) dried (Na2SO4) and concentrated in vacuo. Purification by column chromatography (SiO2, 8 to 10% EtOAc in petroleum ether eluant) gave pure compound 9 (0.72 g, 81%) as gummy syrup.

1. customThe reaction mixture was quenched with 2N NaOH (6 mL) and H2O2 (3 mL) at 0° C.
2. stirringto stir for 4 h
3. customThen crude reaction mixture
4. extractionwas extracted with ethyl acetate (40 mL)
5. washwashed with water (10 mL), brine (10 mL)
6. dry with materialdried (Na2SO4)
7. concentrationconcentrated in vacuo
8. customPurification by column chromatography (SiO2, 8 to 10% EtOAc in petroleum ether eluant)