HRID1709772

反应详情

EQUATION

反应方程式

HRID 1709772 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of 13 g of 5,6-dichloro-2-benzimidazolethiol in 360 ml of alcohol was treated with 13 g of 2-chloromethyl-4-methoxy 3-methylpyridine hydrochloride. A solution of 4 g of sodium hydroxide in 170 ml of water was added dropwise thereto while cooling with ice. The mixture was left to boil at reflux overnight and then concentrated to about 1/3 of its volume in a vacuum. After the addition of 600 ml of water the crystals were filtered off and thereupon washed thoroughly with water and then with ether. There was obtained 5,6-dichloro-2-[[(4-methoxy-3-methyl-2-pyridyl)methyl]thio]benzimidazole of melting point 254°-256°.

WORKUP

后处理

  1. temperaturewhile cooling with ice
  2. waitThe mixture was left
  3. temperatureat reflux overnight
  4. concentrationconcentrated to about 1/3 of its volume in a vacuum
  5. additionAfter the addition of 600 ml of water the crystals
  6. filtrationwere filtered off
  7. washwashed thoroughly with water