HRID1080660

反应详情

EQUATION

反应方程式

HRID 1080660 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A solution of hydrogen chloride in ether is added to a solution of 3.4 g of 3-tetrahydropyranyloxyethyl-3-(3,4-dichlorophenyl)pyrrolidine in 20 ml of methanol until the pH is 1. The mixture is stirred for half an hour at room temperature and concentrated to dryness, the residue is taken up in water, rendered basic with a solution of sodium hydroxide and extracted with dichloromethane and the extract is washed with a saturated solution of NaCl, dried over Na2SO4 and evaporated to dryness to give an oil. This oil is taken up in 20 ml of an isopropyl ether/ether mixture (50/50 v/v). After stirring and filtration, the product is washed with ethyl ether and dried under vacuum over P2O5. 2.6 g of the expected product are isolated.

WORKUP

后处理

  1. concentrationconcentrated to dryness
  2. extractionextracted with dichloromethane
  3. washthe extract is washed with a saturated solution of NaCl
  4. dry with materialdried over Na2SO4
  5. customevaporated to dryness
  6. customto give an oil
  7. stirringAfter stirring
  8. filtrationfiltration
  9. washthe product is washed with ethyl ether
  10. dry with materialdried under vacuum over P2O5