反应详情

温度

0 °C

To the stirred solution of compound 6 (1.3 g, 4.77 mmol) in dry THF (10 mL) was added LAH (0.212 g, 5.73 mmol) at −78° C. under argon atmosphere and stirred the reaction mixture for 3 h then the reaction mixture was warmed to 0° C. and quenched with ethyl acetate (30 mL) at 0° C. After the reaction mixture was back to room temperature, extracted with 2M potassium sodium tartrate solution, washed with, brine (20 mL) dried (Na2SO4) and concentrated in vacuo. Purification by column chromatography (SiO2, 15 to 20% EtOAc in petroleum ether eluant) gave pure compound 7 (0.88 g, 80%) as gummy syrup.

1. customquenched with ethyl acetate (30 mL) at 0° C
2. customwas back to room temperature
3. extractionextracted with 2M potassium sodium tartrate solution
4. washwashed with, brine (20 mL)
5. dry with materialdried (Na2SO4)
6. concentrationconcentrated in vacuo
7. customPurification by column chromatography (SiO2, 15 to 20% EtOAc in petroleum ether eluant)