HRID544649

反应详情

EQUATION

反应方程式

HRID 544649 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

0.217 g of ethyl mercaptan is dissolved under nitrogen in 10 ml of hexamethylphosphoric acid triamide, the solution is cooled to 10° and, while stirring, 170 mg of 50% strength sodium hydride suspension (in mineral oil, de-oiled with hexane) are added in portions. The mixture is then stirred for 15 minutes at room temperature, 1.0 g of 2-chloro-4,5-bis-(p-methoxyphenyl)-thiazole is added and stirring is carried out at room temperature for 1 hour. The mixture is then poured into 300 ml of 10% strength sodium chloride solution, digested until crystallisation occurs and filtered with suction and the residue is then washed twice with water and sucked dry on a suction filter. The crude product is recrystallised from methanol. 2-Ethylthio-4,5-bis-(p-methoxyphenyl)-thiazole having a melting point of 73°-75° is obtained.

WORKUP

后处理

  1. temperaturethe solution is cooled to 10°
  2. stirringThe mixture is then stirred for 15 minutes at room temperature
  3. stirringstirring
  4. customdigested until crystallisation
  5. filtrationfiltered with suction
  6. washthe residue is then washed twice with water
  7. customsucked dry on a suction
  8. filtrationfilter
  9. customThe crude product is recrystallised from methanol