HRID1257441

反应详情

EQUATION

反应方程式

HRID 1257441 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-78 °C

PROCEDURE

实验过程

The compound (0.83 g) obtained in Example 129a was dissolved in tetrahydrofuran (15 mL), cooled to −78° C., and n-butyllithium (2.5M hexane solution, 1.24 mL) was added. The mixture was stirred at the same temperature for 1 hr, N,N-dimethylformamide (1.0 mL) was added, the reaction mixture was warmed to room temperature and stirred for 1 hr. 1N Hydrochloric acid (20 mL) was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The obtained organic layer was washed with saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure. The residue was purified by column chromatography (carrier: silica gel, eluent: hexane/ethyl acetate) to give the title compound (0.45 g) as a solid.

WORKUP

后处理

  1. temperaturethe reaction mixture was warmed to room temperature
  2. stirringstirred for 1 hr
  3. extractionthe mixture was extracted with ethyl acetate
  4. washThe obtained organic layer was washed with saturated brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customThe solvent was evaporated under reduced pressure
  7. customThe residue was purified by column chromatography (carrier: silica gel, eluent: hexane/ethyl acetate)