HRID747711

反应详情

EQUATION

反应方程式

HRID 747711 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

236 mg (5.9 mmol) of sodium hydride (oily, 60%) was stirred in dimethylformamide. 691 mg (5.8 mmol) of 3-hydroxybenzonitrile was added thereto under cooling with ice. After stirring at room temperature for 30 minutes, a solution of 2 g (5.75 mmol) of 2-(4-bromophenyl)-2-(3-chloropropyl)-5,5-dimethyl-1,3-dioxane in dimethylformamide was added to the reaction mixture, and they were stirred at 100° C. overnight. Water was added to the mixture. After the extraction with ethyl acetate, the organic layer was washed with 1 N aqueous sodium hydroxide solution and saturated aqueous common salt solution and dried over anhydrous magnesium sulfate. The solvent was evaporated to obtain the crude title compound.

WORKUP

后处理

  1. temperatureunder cooling with ice
  2. stirringwere stirred at 100° C. overnight
  3. extractionAfter the extraction with ethyl acetate
  4. washthe organic layer was washed with 1 N aqueous sodium hydroxide solution and saturated aqueous common salt solution
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customThe solvent was evaporated