HRID1857210

反应详情

EQUATION

反应方程式

HRID 1857210 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4-Cyclohexylcarbonyl-1-methoxybenzene (517 mg) obtained in Example 141 was dissolved in N,N-dimethylformamide (20 ml), sodium thiomethoxide (538 mg) was added, and the admixture was refluxed with heat for 1 hour under argon. The reaction mixture was partitioned between water and ethyl acetate, and the ethyl acetate layer was washed with brine and then dried with anhydrous sodium sulfate. After removing the solvent by reduced-pressure distillation, the resulting residue was purified by chromatography on silica gel eluting with hexane/acetone to obtain 487 mg of the title compound (yield: 93%).

WORKUP

后处理

  1. temperaturethe admixture was refluxed
  2. temperaturewith heat for 1 hour under argon
  3. customThe reaction mixture was partitioned between water and ethyl acetate
  4. washthe ethyl acetate layer was washed with brine
  5. dry with materialdried with anhydrous sodium sulfate
  6. customAfter removing the solvent
  7. distillationby reduced-pressure distillation
  8. customthe resulting residue was purified by chromatography on silica gel eluting with hexane/acetone