HRID34276

反应详情

EQUATION

反应方程式

HRID 34276 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 2-(4-methyl-1-piperazinyl)acetic acid, hydrazide (3.44 g., 0.020 mole) and 3,5-difluorobenzylisothiocyanate (3.70 g., 0.020 mole) in ethanol (40 ml.) was refluxed for 17 hours and the solvent was removed under vacuum. The residue was triturated with ethyl acetate-ether and the resulting solid was filtered and recrystallized twice from ethanol to give 3-mercapto-4-(3, 5-difluorobenzyl)-5-[(4-methyl-1-piperazinyl)methyl]-1,2,4-triazole as a solid melting at 200°-201° C. (4.60 g., 68%).

WORKUP

后处理

  1. customthe solvent was removed under vacuum
  2. customThe residue was triturated with ethyl acetate-ether
  3. filtrationthe resulting solid was filtered
  4. customrecrystallized twice from ethanol