HRID979453

反应详情

EQUATION

反应方程式

HRID 979453 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 59.2 g (0.47 mole) of dimethyl sulphate and 32 g (0.517 mole) of dimethyl sulphide in 270 ml of acetonitrile is allowed to stir at room temperature for 5 days. Then, at 20° to 25° C., a solution of 87 g of 4-chlorophenyl 2-(p-chlorophenoxy)-2-propyl ketone in 80 ml of acetonitrile is added dropwise within about 2 hours. At the same temperature, 28.7 g (0.53 mole) of sodium methylate are added, the mixture is allowed to stir for 12 hours and then evaporated. The residue is vigorously stirred with a mixture of 200 ml of ethyl acetate and 150 ml of water overnight. The organic phase is separated off, dried over sodium sulphate and evaporated in vacuo. 49 g (76% of theory) of crude 2-(4-chlorophenyl)-2-[2-(p-chlorophenoxy)-2-propyl]oxirane are obtained, and this is immediately reacted further. ##STR47##

WORKUP

后处理

  1. stirringto stir for 12 hours
  2. customevaporated
  3. stirringThe residue is vigorously stirred with a mixture of 200 ml of ethyl acetate and 150 ml of water overnight
  4. customThe organic phase is separated off
  5. dry with materialdried over sodium sulphate
  6. customevaporated in vacuo