HRID725722

反应详情

EQUATION

反应方程式

HRID 725722 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

5,6-dichloro-2-mercaptobenzimidazole (8.76 g, 0.04 mol) in 50 ml 95% ethanol was treated with 10 ml of 45% aqueous potassium hydroxide to give a solution. Iodomethane (7 ml, 0.096 mol) was added. The reaction mixture was refluxed for two hours. Cooling overnight yielded precipitant, which was filtered, water-washed, and dried to yield 5.61 g, mp 115° C. The reaction filtrate was rotary evaporated and the residue reslurried in water. After filtration and drying, an additional 3.52 g was obtained, mp 110° C. NMR analysis indicated the presence of some 5,6-DiChloro-2-(methylthio)benzimidazole as an impurity.

WORKUP

后处理

  1. customto give a solution
  2. temperatureThe reaction mixture was refluxed for two hours
  3. temperatureCooling overnight
  4. customyielded precipitant
  5. filtrationwhich was filtered
  6. washwater-washed
  7. customdried
  8. customto yield 5.61 g, mp 115° C
  9. customThe reaction filtrate was rotary evaporated
  10. filtrationAfter filtration
  11. customdrying
  12. customan additional 3.52 g was obtained