HRID1597394

反应详情

EQUATION

反应方程式

HRID 1597394 的结构方程式

PROCEDURE

实验过程

To a stirred solution of (R)-1-benzyl-3-pyrrolidinol (886 mg, 5.0 mmol) in CCl4(20 ml) was added triphenylphosphine(1.574 g, 6.0 mmol) at rt. After 20 h stirring at reflux temperature, the solvent was evaporated. Saturated NaHCO3 aqueous solution and water was added to the residue, and the mixture was extracted with AcOEt. The extract was brine, dried(Na2SO4), and concentrated to give brown oil, which was purified by column chromatography (silica gel; 100 g, CH2Cl2/MeOH: 50/1-45/1) to give 706 mg(72%) of pale yellow oil.

WORKUP

后处理

  1. temperatureat reflux temperature
  2. customthe solvent was evaporated
  3. additionSaturated NaHCO3 aqueous solution and water was added to the residue
  4. extractionthe mixture was extracted with AcOEt
  5. concentrationconcentrated
  6. customto give brown oil, which
  7. customwas purified by column chromatography (silica gel; 100 g, CH2Cl2/MeOH: 50/1-45/1)