HRID4904

反应详情

EQUATION

反应方程式

HRID 4904 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

13.8 g of potassium carbonate and 50 ml of DMF were placed in a 200 ml eggplant type flask, and 11.1 g of methyl 2-formyl-6-hydroxybenzoate and 14.6 g of 4,6-dimethoxy-2-methanesulfonylpyrimidine were added thereto with stirring. The mixture was stirred at 80° C. for 1 hour, and the resultant liquor was poured into an ice water after cooling. An oily product thus precipitated was extracted with ethyl acetate, and was dried with magnesium sulfate anhydride. Ethyl acetate was distilled off under reduced pressure, and the residue thus obtained was purified by column chromatography to obtain 11.0 g of the aimed compound (melting point=91° to 93° C.) at a yield of 52%.

WORKUP

后处理

  1. stirringThe mixture was stirred at 80° C. for 1 hour
  2. temperatureafter cooling
  3. customAn oily product thus precipitated
  4. extractionwas extracted with ethyl acetate
  5. dry with materialwas dried with magnesium sulfate anhydride
  6. distillationEthyl acetate was distilled off under reduced pressure
  7. customthe residue thus obtained
  8. customwas purified by column chromatography