HRID1709758

反应详情

EQUATION

反应方程式

HRID 1709758 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

10.6 g of 5-fluoro-2-benzimidazolethiol were suspended in 570 ml of alcohol and treated with 13.1 g of 2-chloromethyl-4-methoxy-3-methylpyridine hydrochloride. A solution of 5 g of sodium hydroxide in 130 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 the volume in a vacuum. After the addition of 500 ml of water the resulting crystals were filtered off and washed thoroughly firstly with water and then with ether. There was obtained 5-fluoro-2-[[(4-methoxy-3-methyl-2-pyridyl)methyl]thio]benzimidazole of melting point 128°.

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 the volume in a vacuum
  5. additionAfter the addition of 500 ml of water the resulting crystals
  6. filtrationwere filtered off
  7. washwashed thoroughly firstly with water