HRID1073030

反应详情

EQUATION

反应方程式

HRID 1073030 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

10.4 g of 2-mercapto-4,6-dimethoxypyrimidine, 15.0 g of ethyl 2-(1-cyclopentenyl)-2-(methylsulfonyloxy)acetate, 100 ml of N,N-dimethylformamide and 9.2 g of anhydrous potassium carbonate were stirred at 90° C. for 5 hours. The reaction mixture was cooled to room temperature and then diluted with water. The aqueous mixture was extracted with ethyl ether. The ethyl ether extract was washed with water and dried. Then, ethyl ether was removed by distillation under reduced pressure to obtain an yellow oily substance. The yellow oily substance was purified by silica gel column chromatography (eluent: hexane/ethyl acetate =10/1) to obtain 9.7 g of the desired product.

WORKUP

后处理

  1. extractionThe aqueous mixture was extracted with ethyl ether
  2. extractionThe ethyl ether extract
  3. washwas washed with water
  4. customdried
  5. customThen, ethyl ether was removed by distillation under reduced pressure
  6. customto obtain an yellow oily substance
  7. customThe yellow oily substance was purified by silica gel column chromatography (eluent: hexane/ethyl acetate =10/1)