反应详情

温度

-78 °C

To a solution of compound 4A (898 mg, 2.50 mmol) in THF (10 mL) at −78° C. under nitrogen was added a 1.8 M solution of LDA (3.50 mL, 6.25 mmol) and the reaction was stirred at −78° C. for 1 h. Iodomethane (1.56 mL, 25.0 mmol) was added, and the mixture was stirred at −78° C. for 4 h. The reaction was quenched by adding EtOAc and water. The layers were separated and the aqueous layer was extracted with EtOAc (3×20 mL). The combined organic layers were washed with saturated aqueous NaHCO3 and brine, then dried over MgSO4, filtered and concentrated. Purification via silica gel chromatography (0-15% EtOAc in hexane) provided compound 4B (276 mg).

1. stirringthe mixture was stirred at −78° C. for 4 h
2. customThe reaction was quenched
3. additionby adding EtOAc and water
4. customThe layers were separated
5. extractionthe aqueous layer was extracted with EtOAc (3×20 mL)
6. washThe combined organic layers were washed with saturated aqueous NaHCO3 and brine
7. dry with materialdried over MgSO4
8. filtrationfiltered
9. concentrationconcentrated
10. customPurification via silica gel chromatography (0-15% EtOAc in hexane)