HRID1954455

反应详情

EQUATION

反应方程式

HRID 1954455 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

186 g of 3-(2-cyclohexylthio-thiazol-5-yl-methyl)-5-methyl-4-nitroimino-perhydro-1,3,5-oxadiazine are introduced over a period of 5 minutes, with stirring, into a mixture of 300 g of hydrochloric acid (32%) and 150 g of chlorobenzene. 124 g of chlorine are introduced at 20° C. over a period of 4 hours. After 2 hours, excess chlorine is removed by the introduction of nitrogen, and the phases are then separated. The aqueous phase is adjusted to pH 5 with sodium hydroxide solution (30%) and then filtered, and the filtration residue is washed with water and dried in vacuo at 50° C. The title product is obtained in a purity of 97%.

WORKUP

后处理

  1. customexcess chlorine is removed by the introduction of nitrogen
  2. customthe phases are then separated
  3. filtrationfiltered
  4. washthe filtration residue is washed with water
  5. customdried in vacuo at 50° C