HRID341761

反应详情

EQUATION

反应方程式

HRID 341761 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 24.4 g of N-(4-methoxy-phenyl)-3,3-dimethyl-4-phenylazetidin-2-one and 16.5 g of lithium 25 perchlorate in a mixture of 500 cm3 of acetonitrile and 50 cm3 of water, is subjected to electrolysis in a unseparated cell, using a graphite anode and a stainless steel grille as cathode and maintaining a constant potential difference of 1.5 V. At the end of the reaction the solution is concentrated to 1/4 of volume. An extraction is made with ethyl acetate and the organic phase is washed with a solution of aqueous sodium sulphite at 10% and then with water; it is dried with sodium sulphate and then evaporated. The raw product is purified on silica gel, using a mixture of ethyl acetate/hexane as eluant in a ratio of 3/7 and 15.4 g of 3,3-dimethyl-4-phenylazetidin-2-one are obtained (yield (98%).

WORKUP

后处理

  1. customAt the end of the reaction the solution
  2. concentrationis concentrated to 1/4 of volume
  3. extractionAn extraction
  4. washthe organic phase is washed with a solution of aqueous sodium sulphite at 10%
  5. dry with materialit is dried with sodium sulphate
  6. customevaporated
  7. customThe raw product is purified on silica gel
  8. additiona mixture of ethyl acetate/hexane as eluant in a ratio of 3/7 and 15.4 g of 3,3-dimethyl-4-phenylazetidin-2-one
  9. customare obtained (
  10. customyield (98%)