HRID981574

反应详情

EQUATION

反应方程式

HRID 981574 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of N-(3,5-difluoro-4-methoxybenzyl)-aminoacetaldehyde dimethyl acetal (4.94 g, 0.0189 mole) in ethyl alcohol (30 ml) was added potassium thiocyanate (2.10 g, 0.0216 mole) in water (48 ml) followed by 12 N hydrochloric acid (4 ml), and the reaction mixture was heated under reflux for 3.5 hours. The solvent was partially removed under reduced pressure, the mixture was cooled in ice, and the product was filtered. The product was recrystallized from ethyl alcohol - hexane to give 1-(3,5-difluoro-4-methoxybenzyl)-2-mercaptoimidazole as a solid melting at 160-161° (2.22 g, 46%).

WORKUP

后处理

  1. temperaturethe reaction mixture was heated
  2. temperatureunder reflux for 3.5 hours
  3. customThe solvent was partially removed under reduced pressure
  4. temperaturethe mixture was cooled in ice
  5. filtrationthe product was filtered
  6. customThe product was recrystallized from ethyl alcohol - hexane