HRID1871943

反应详情

EQUATION

反应方程式

HRID 1871943 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-{[[4-(2-Furylmethylthio)-3-methyl-2-pyridinyl]methyl]thio}-1H-benzimidazole is stirred with 2-dimethylamino-ethyl chloride hydrochloride (1.5 equivalents), potassium carbonate (5 equivalents) and potassium iodide (0.05 equivalents) in acetonitrile at 100° C. for 24 h, the mixture is filtered, the filtrate is concentrated on a rotary evaporator, water is added to the residue and the mixture is extracted with methylene chloride. The combined organic phases are washed with water, dried and concentrated. The residue is crystallized from methylene chloride/diisopropyl ether. The title compound is obtained as a colorless powder; m.p. 87-89° C.; yield: 74% of theory.

WORKUP

后处理

  1. filtrationthe mixture is filtered
  2. concentrationthe filtrate is concentrated on a rotary evaporator, water
  3. additionis added to the residue
  4. extractionthe mixture is extracted with methylene chloride
  5. washThe combined organic phases are washed with water
  6. customdried
  7. concentrationconcentrated
  8. customThe residue is crystallized from methylene chloride/diisopropyl ether