HRID462340

反应详情

EQUATION

反应方程式

HRID 462340 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

To a solution of 10.8 g of sodium methylate in 50 ml of methanol are added 28.9 g of 2-amino-4-(3-chloropropyl)-6-trichloromethyl-1,3,5-triazine, and the mixture is stirred at 60° C. for 80 minutes. The formed suspension is filtered under suction, diluted with 250 ml of water, and extracted 3 times with 200 ml of ethylene chloride each time. The organic phases are dried, filtered, and concentrated by evaporation. The oil which remains is purified through a silica gel column, the eluant used being methylene chloride/ether (3:1). The eluant is evaporated off to leave 2.1 g of the title product, which is recrystallised from ether/chloroform, m.p. 158°-159° C.

WORKUP

后处理

  1. filtrationThe formed suspension is filtered under suction
  2. additiondiluted with 250 ml of water
  3. extractionextracted 3 times with 200 ml of ethylene chloride each time
  4. customThe organic phases are dried
  5. filtrationfiltered
  6. concentrationconcentrated by evaporation
  7. customThe oil which remains is purified through a silica gel column
  8. customThe eluant is evaporated off