HRID876349

反应详情

EQUATION

反应方程式

HRID 876349 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

54.6 mg of pyridinium p-toluenesulphonate (0.217 mmol) were added to a solution of the acetal from Example 64A (400 mg, 0.725 mmol) in 15 ml of acetone/water (10:1) and the mixture was stirred under reflux for 3 d, with another 54.6 mg of pyridinium p-toluenesulphonate (0.217 mmol) being added after 24 h and 48 h. The solvent was then removed under reduced pressure, the residue was taken up in water and the mixture was extracted with dichloromethane. The organic phase was dried over magnesium sulphate, filtered and concentrated under reduced pressure. Yield: 363 mg (92% of theory)

WORKUP

后处理

  1. additionbeing added after 24 h and 48 h
  2. customThe solvent was then removed under reduced pressure
  3. extractionthe mixture was extracted with dichloromethane
  4. dry with materialThe organic phase was dried over magnesium sulphate
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure