HRID1828396

反应详情

EQUATION

反应方程式

HRID 1828396 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To the above slurry of (butylmethylene) triphenylphosphorane at 10° C. under an argon atmosphere was added dropwise a solution of (3,5-dimethoxyphenyl)cyclopentane carboxaldehyde (1 equiv.) in dry THF (0.21M). The reaction was stirred for 45 min and upon completion was quenched by the addition of saturated aqueous ammonium chloride. The organic layer was separated and the aqueous phase was extracted twice with diethyl ether. The combined organic layer was washed with brine, dried over MgSO4 and the solvent was evaporated under reduced pressure to give an oil. The crude product was purified through a short column of silica gel using 5% diethyl ether-petroleum ether as eluent to afford the title compound in 96% yield.

WORKUP

后处理

  1. customwas quenched by the addition of saturated aqueous ammonium chloride
  2. customThe organic layer was separated
  3. extractionthe aqueous phase was extracted twice with diethyl ether
  4. washThe combined organic layer was washed with brine
  5. dry with materialdried over MgSO4
  6. customthe solvent was evaporated under reduced pressure
  7. customto give an oil
  8. customThe crude product was purified through a short column of silica gel using 5% diethyl ether-petroleum ether as eluent