反应详情

温度

-78 °C

To a solution of Intermediate 12.1 (50.0 mg, 0.263 mmol) in 2 mL THF at −78° C. was added 1.6 M solution of BuLi in THF (181 μL, 0.289 mmol). The mixture was stirred at −78° C. for 2 min, then a solution of Intermediate 7.3 (86 mg, 0.263 mmol) in 0.6 mL THF was added dropwise. The mixture was stirred at −78° C. for 30 min, was allowed to warm to rt over 1 h, then was quenched with sat. NH4Cl. The mixture was diluted with EtOAc, washed with H2O and brine, dried (Na2SO4) and concentrated. The crude product was purified by flash chromatography (25 to 30% EtOAc/hexanes, stepwise gradient) to afford 33 mg of Intermediate 12.2 as yellow residue.

1. stirringThe mixture was stirred at −78° C. for 30 min
2. temperatureto warm to rt over 1 h
3. customwas quenched with sat. NH4Cl
4. additionThe mixture was diluted with EtOAc
5. washwashed with H2O and brine
6. dry with materialdried (Na2SO4)
7. concentrationconcentrated
8. customThe crude product was purified by flash chromatography (25 to 30% EtOAc/hexanes, stepwise gradient)