HRID1027712

反应详情

EQUATION

反应方程式

HRID 1027712 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3.2 g of 5-amino-2,4-dichloropyrimidine in 50 ml ethyl acetate were added to a mixture of 25 ml of saturated aqueous sodium bicarbonate solution and 25 ml of water. At room temperature, a solution of 4.9 g of 3,5-dimethyl-4-methoxybenzoyl chloride was added over a period of 15 min. The mixture was stirred intensively for 4 h. The layers were then separated, after which the aqueous layer was extracted twice with ethyl acetate. After drying over sodium sulfate and filtration, the solvent was removed under reduced pressure, giving 7.54 g of crude product. The crude product was triturated with 25 ml of isopropanol. Filtration and washing with 10 ml of isopropanol gave 2.74 g of the title compound in the form of a white solid.

WORKUP

后处理

  1. customThe layers were then separated
  2. extractionafter which the aqueous layer was extracted twice with ethyl acetate
  3. dry with materialAfter drying over sodium sulfate and filtration
  4. customthe solvent was removed under reduced pressure
  5. customgiving 7.54 g of crude product
  6. customThe crude product was triturated with 25 ml of isopropanol
  7. filtrationFiltration
  8. washwashing with 10 ml of isopropanol