HRID1957489

反应详情

EQUATION

反应方程式

HRID 1957489 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To methylene chloride, 47.5 g of aluminum chloride were added, followed by the addition of 30 g of 2,4,5-trimethoxybenzene and then 13 ml of acetyl chloride under ice cooling. The resulting mixture was stirred at room temperature for 6 hours. After the completion of the reaction, 1N hydrochloric acid was added to the reaction mixture under ice cooling. The resulting mixture was then extracted with methylene chloride. The extract so obtained was washed successively with 1N hydrochloric acid, a 1N aqueous solution of sodium hydrochloride and saturated saline and then dried over anhydrous magnesium sulfate. The organic layer was concentrated under reduced pressure. The crude product so obtained was washed with ethanol, whereby 18.6 g of 2',4',5'-trimethoxyacetophenone were obtained (yield: 50%).

WORKUP

后处理

  1. additionwas added to the reaction mixture under ice cooling
  2. extractionThe resulting mixture was then extracted with methylene chloride
  3. extractionThe extract so
  4. customobtained
  5. washwas washed successively with 1N hydrochloric acid
  6. dry with materiala 1N aqueous solution of sodium hydrochloride and saturated saline and then dried over anhydrous magnesium sulfate
  7. concentrationThe organic layer was concentrated under reduced pressure
  8. customThe crude product so obtained
  9. washwas washed with ethanol