反应详情

温度

0 °C

To a solution of Compound 150 (0.17 g, 0.81 mmol) in Et2O (5.0 mL) at −78° C. under Argon atmosphere was added dropwise a solution of 1.7M t-BuLi in pentane (1.0 mL, 1.79 mmol), and the reaction was stirred for 1 h. DMF (0.25 mL, 3.24 mmol) was added, and the cooling bath was removed. After 1h15, the reaction was cooled to 0° C., and saturated NH4Cl was added. The mixture was extracted with EtOAc, washed with brine, dried over MgSO4, and filtered. The solvent was removed, and the residue was purified by silica gel flash chromatography with EtOAc (15%) and hexanes (85%) as eluent to produce Compound 151 as a yellow oil.

1. customthe cooling bath was removed
2. additionsaturated NH4Cl was added
3. extractionThe mixture was extracted with EtOAc
4. washwashed with brine
5. dry with materialdried over MgSO4
6. filtrationfiltered
7. customThe solvent was removed
8. customthe residue was purified by silica gel flash chromatography with EtOAc (15%) and hexanes (85%) as eluent