HRID1380826

反应详情

EQUATION

反应方程式

HRID 1380826 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
45 °C

PROCEDURE

实验过程

8.0 g (0.043 mol) of 6-ethoxy-4-chloromethyl-2-methyl-pyrimidine and 10.8 g (0.045 mol) of potassium O-ethyl S-(n-propyl) dithiophosphate are suspended in 20 ml of acetone. After the addition of a small amount (spatula tip) of sodium iodide the mixture is stirred well at 45° C. for 12 hours. The mixture is then filtered through Celite, the filtrate is concentrated under reduced pressure and the thus-isolated solid is taken up in 100 ml of toluene. The toluene solution is washed once with 5% sodium carbonate solution and once with saturated sodium chloride solution and dried over anhydrous sodium sulphate, and the solvent is removed by evaporation at 60° C. under reduced pressure. In this manner there is obtained O-ethyl S-(6-ethoxy-2-methyl-4-pyrimidinylmethyl) S-(n-propyl) dithiophosphate as an almost colourless oil, nD20 1.5385.

WORKUP

后处理

  1. filtrationThe mixture is then filtered through Celite
  2. concentrationthe filtrate is concentrated under reduced pressure
  3. washThe toluene solution is washed once with 5% sodium carbonate solution and once with saturated sodium chloride solution
  4. dry with materialdried over anhydrous sodium sulphate
  5. customthe solvent is removed by evaporation at 60° C. under reduced pressure