HRID1031976

反应详情

EQUATION

反应方程式

HRID 1031976 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4-Methanesulphonamidophenethyl mesylate (10 g, 34 mmole) and N-ethylbenzylamine (10 ml, 67 mmole) were heated at reflux temperature in ethanol (80 ml) for 3 hours. The solvent was evaporated, the residue taken up in 2M hydrochloric acid and washed twice with methylene chloride. The aqueous layer was basified with sodium bicarbonate (to pH~12) and extracted with methylene chloride. The latter organic extract was dried (MgSO4) and evaporated to give an oil which solidified when triturated with diisopropyl ether. The solid was filtered off and discarded and the filtrate was evaporated in vacuo to give the title compound as an oil, yield 4.4 g.

WORKUP

后处理

  1. customThe solvent was evaporated
  2. washwashed twice with methylene chloride
  3. extractionextracted with methylene chloride
  4. extractionThe latter organic extract
  5. dry with materialwas dried (MgSO4)
  6. customevaporated
  7. customto give an oil which
  8. customtriturated with diisopropyl ether
  9. filtrationThe solid was filtered off
  10. customthe filtrate was evaporated in vacuo