HRID1739506

反应详情

EQUATION

反应方程式

HRID 1739506 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 5-ethyl-2-trifluoroacetylamino-1,3,4-thiadiazole (22.5 g) and 4-iodobenzyl bromide (32.7 g) in N,N-dimethylformamide (100 ml) was added potassium carbonate (13.8 g), followed by stirring at room temperature overnight. To the reaction mixture, ethyl acetate (500 ml) was added. The resulting mixture was washed three times with 10% aqueous citric acid solution, followed by drying over anhydrous magnesium sulfate. The solvent was then distilled off. The oily substance so obtained was separated by column chromatography on silica gel. The crystals so obtained were dispersed in n-hexane, collected by filtration and then dried, whereby 33.9 g of the title compound was obtained.

WORKUP

后处理

  1. washThe resulting mixture was washed three times with 10% aqueous citric acid solution
  2. dry with materialby drying over anhydrous magnesium sulfate
  3. distillationThe solvent was then distilled off
  4. customThe oily substance so obtained
  5. customwas separated by column chromatography on silica gel
  6. customThe crystals so obtained
  7. filtrationcollected by filtration
  8. customdried