反应详情

温度

-78 °C

To a solution of compound 1a (14 g, 29.6 mmol) in dry THF (500 ml) at −78° C. was added dropwise n-BuLi (18.5 mL, 1.6 M in hexane, 29.6 mmol). The mixture was stirred for an additional 1 h at −78° C. and a solution of compound 2a (6.5 g, 28.9 mmol) in dry THF (50 mL) was added dropwise. The resulting mixture was stirred at −78° C. for 1 h and then warmed to rt and quenched with saturated aq. NH4Cl (500 mL). The mixture was extracted with EA (500 mL×2), the combined organic layers were washed with brine, dried over Na2SO4 and concentrated in vacuo. The residue was purified by CC (EA/PE=1:5) to give the title compound 2b (6.5 g, 37%) as a white solid.

1. stirringThe resulting mixture was stirred at −78° C. for 1 h
2. temperaturewarmed to rt
3. customquenched with saturated aq. NH4Cl (500 mL)
4. extractionThe mixture was extracted with EA (500 mL×2)
5. washthe combined organic layers were washed with brine
6. dry with materialdried over Na2SO4
7. concentrationconcentrated in vacuo
8. customThe residue was purified by CC (EA/PE=1:5)