HRID1777361

反应详情

EQUATION

反应方程式

HRID 1777361 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
42.5 °C

PROCEDURE

实验过程

Thionyl chloride (3.1 mL, 0.043 mol) and N,N-dimethylformamide (0.2 mL) are added to a stirred solution of {4-[5-(3-chloro-4-isobutylphenyl)-[1,2,4]-oxadiazol-3-yl]-phenyl}methanol (4.9 g, 0.0143 mol) in dichloromethane (30 mL) at 0° C. The reaction mixture is heated at 40-45° C. and is stirred at this temperature for 30 minutes. It is then cooled to 0-5° C. temperature, treated with demineralized water (3 mL) and neutralized with caustic lye to adjust the pH to 8-9. Finally it is extracted with dichloromethane (2×20 mL) and the combined extract is dried over sodium sulfate. Removal of solvent under reduced pressure gives 5-(3-chloro-4-isobutylphenyl)-3-(4-chloromethylphenyl)-[1,2,4]-oxadiazole.

WORKUP

后处理

  1. temperatureIt is then cooled to 0-5° C. temperature
  2. extractionFinally it is extracted with dichloromethane (2×20 mL)
  3. extractionthe combined extract
  4. dry with materialis dried over sodium sulfate
  5. customRemoval of solvent under reduced pressure