HRID495244

反应详情

EQUATION

反应方程式

HRID 495244 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a flask were added 2 g 2-mercapto-5-methylbenzimidazole, 4.2 g potassium carbonate, 4.0 g 1,3-diiodopropane and 60 ml N,N-dimethylformamide. The mixture was heated to 50 C under nitrogen for 5 hours and then cooled to 22 C. The reaction was quenched with 100 ml water and the product was extracted twice with ethyl acetate and washed twice with water. Following removal of the solvent, the product was recrystallized by dissolving in a hot mixture of 50 ml hexane with 10 ml 2-propanol. After cooling to 5 C, the product was filtered, washed with hexane and dried giving 0.63 g of an off-white solid.

WORKUP

后处理

  1. temperatureThe mixture was heated to 50 C under nitrogen for 5 hours
  2. temperaturecooled to 22 C
  3. customThe reaction was quenched with 100 ml water
  4. extractionthe product was extracted twice with ethyl acetate
  5. washwashed twice with water
  6. customremoval of the solvent
  7. customthe product was recrystallized
  8. dissolutionby dissolving in a hot mixture of 50 ml hexane with 10 ml 2-propanol
  9. temperatureAfter cooling to 5 C
  10. filtrationthe product was filtered
  11. washwashed with hexane
  12. customdried