HRID1388294

反应详情

EQUATION

反应方程式

HRID 1388294 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 4.44 g (0.03 m) of 4-hydroxy-1-indanone in 50 ml of dimethylformamide is added 4.15 g (0.03 m) of potassium carbonate with stirring followed by the dropwise addition of 3.8 g (0.03 m) of benzyl chloride. The reaction mixture is heated at steam bath temperature for 3 hours, then cooled and diluted with water. The aqueous mixture is extracted with ethyl acetate and the extract is washed with water, dried over anhydrous sodium sulfate and concentrated to dryness in vacuo. The residue is triturated with ether and concentrated to dryness to yield: 5.86 g (82%) of a brown solid, m.p. 70°-73° C., sufficiently pure to be used in the next step.

WORKUP

后处理

  1. temperatureThe reaction mixture is heated at steam bath temperature for 3 hours
  2. temperaturecooled
  3. extractionThe aqueous mixture is extracted with ethyl acetate
  4. washthe extract is washed with water
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationconcentrated to dryness in vacuo
  7. customThe residue is triturated with ether
  8. concentrationconcentrated to dryness to yield: 5.86 g (82%) of a brown solid, m.p. 70°-73° C.