反应详情

温度

-78 °C

The compound prepared in Example 96 (0.050 g) was suspended in dry tetrahydrofuran (10 mL) and cooled to −78° C. n-Butyl lithium (2.5 mol/L solution in hexane, 0.03 mL) was added dropwise and the reaction was allowed to stirred at −78° C. for 5 minutes. A saturated aqueous ammonium chloride solution was added and the reaction mixture was warmed to room temperature. The mixture was partitioned between a saturated aqueous ammonium chloride solution and ethyl acetate. The organics were washed with brine, dried over anhydrous magnesium sulfate and concentrated. The residue was purified by column chromatography on silica gel to obtain the title compound (0.015 g) having the following physical data.

1. additionwas added dropwise
2. temperaturethe reaction mixture was warmed to room temperature
3. customThe mixture was partitioned between a saturated aqueous ammonium chloride solution and ethyl acetate
4. washThe organics were washed with brine
5. dry with materialdried over anhydrous magnesium sulfate
6. concentrationconcentrated
7. customThe residue was purified by column chromatography on silica gel