HRID1651085

反应详情

EQUATION

反应方程式

HRID 1651085 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 5.0 g (0.014 mol) of 1,1-dichloro-3-(4-chlorophenyl)-3-hydroxy-4-(1,2,4-(1H)-triazolyl)butane and 3.85 g (0.043 mol) of sodium 1,2,4-triazolide in 75 mL of dimethylformamide was stirred at room temperature for 28 hours. To this solution was added 200 mL of water and 200 mL of diethyl ether. The organic phase was separated from the aqueous phase and then washed thrice with 100 mL portions of water and then dried over anhydrous sodium sulfate. The solvent was removed by evaporation under reduced pressure to give a yellow oil which solidified on standing overnight. This material was recrystallized from benzene to give the above named product in a yield of 2.6 g (58 percent of theoretical), melting at 95°-99° C.

WORKUP

后处理

  1. customThe organic phase was separated from the aqueous phase
  2. washwashed thrice with 100 mL portions of water
  3. dry with materialdried over anhydrous sodium sulfate
  4. customThe solvent was removed by evaporation under reduced pressure
  5. customto give a yellow oil which
  6. customThis material was recrystallized from benzene
  7. customto give the above named product in a yield of 2.6 g (58 percent of theoretical), melting at 95°-99° C.