反应详情

温度

-78 °C

A solution of 1.3M s-BuLi in cyclohexane (21.8 mL, 28.3 mmol) was added dropwise to a dry ice/acetone cooled solution of the compound of example e (4.6 g, 21.7 mmol) in THF (60 mL), maintaining the internal reaction temperature ≤-65° C. This mixture was stirred at -78° C. for 45 min, then was quenched by the dropwise addition of a solution of trimethylchlorogermane (5.0 g, 32.6 mmol) in THF (30 mL), again maintaining the internal reaction temperature ≤-65° C. The reaction was warmed to 0° C., diluted with ether, and extracted with 10% HCl (2×) followed with sat aq NaHCO3. The ether was dried (MgSO4), concentrated, and purified by HPLC with 6% EtOAc in hexanes to afford 3.2 g of the title compound as a white solid, a 45% yield. m.p. 47°-48° C.

1. temperaturemaintaining the internal reaction temperature ≤-65° C
2. temperatureagain maintaining the internal reaction temperature ≤-65° C
3. temperatureThe reaction was warmed to 0° C.
4. extractionextracted with 10% HCl (2×)
5. dry with materialThe ether was dried (MgSO4)
6. concentrationconcentrated
7. custompurified by HPLC with 6% EtOAc in hexanes