反应详情

温度

-78 °C

To a solution of Compound 10a (50 mg; 0.1 mmol) in tetrahydrofuran (5 mL), cooled to −78° C., was added acetyl chloride (0.009 mL; 0.12 mmol) and triethylamine (0.035 mL; 0.25 mmol). The mixture was stirred at −78° C. for 1 hour. Diluted the resulted mixture with EtOAc and H2O. The organic phase was washed sequentially with H2O, and then dried over Na2SO4. The mixture was filtered and the filtrate was evaporated under reduced pressure to give the crude material. The crude material was purified by flash column chromatography (SiO2), eluting with a EtOAc-heptane gradient to afford Compound 10b (43 mg; 80% yield). MS: m/z 536.0 (M+H)+.

1. washThe organic phase was washed sequentially with H2O
2. dry with materialdried over Na2SO4
3. filtrationThe mixture was filtered
4. customthe filtrate was evaporated under reduced pressure
5. customto give the crude material
6. customThe crude material was purified by flash column chromatography (SiO2)
7. washeluting with a EtOAc-heptane gradient