HRID495228

反应详情

EQUATION

反应方程式

HRID 495228 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 2.0 g 2-mercapto-5-methylbenzimidazole, 4.2 g potassium carbonate, 30 ml N,N-dimethylformamide and 3.9 g benzyl chloride. The reaction mixture was heated to 60 C for 16 hours, then cooled to 50 C and quenched with 60 ml water and cooled to 5 C. The solid was filtered and washed with water and then recrystallized by dissolving in 50 ml hot acetonitrile and adding 10 ml of water. After cooling to 5 C, the product was filtered, washed and dried resulting in 3.5 g white solid as a mixture of the 5-methyl and 6-methyl isomers.

WORKUP

后处理

  1. temperatureThe reaction mixture was heated to 60 C for 16 hours
  2. temperaturecooled to 50 C
  3. customquenched with 60 ml water
  4. temperaturecooled to 5 C
  5. filtrationThe solid was filtered
  6. washwashed with water
  7. customrecrystallized
  8. dissolutionby dissolving in 50 ml hot acetonitrile
  9. additionadding 10 ml of water
  10. temperatureAfter cooling to 5 C
  11. filtrationthe product was filtered
  12. washwashed
  13. customdried