HRID521687

反应详情

EQUATION

反应方程式

HRID 521687 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A mixture of 0.52 g of 2-ethylsulfanylphenylboronic acid pinacol ester, 0.56 g of 6-bromo-5-methyl-2-trifluoromethylimidazo[1,2-a]pyridine, 0.02 g of tris(dibenzylideneacetone)dipalladium(0), 0.05 g of 2-dicyclohexylphosphino-2′,4′,6′-triisopropylphenyl, 0.84 g of tripotassium phosphate and 6 ml of 1,4-dioxane was stirred under heat-reflux for 3 hours. 0.1 ml of water was added to the cooled reaction mixture, and the mixture was stirred under heat-reflux for 5 hours. Ethyl acetate and water were added to the cooled reaction mixture, and the mixture was filtered. The filtrate was extracted with ethyl acetate and then dried over anhydrous sodium sulfate. The dried matter was concentrated under reduced pressure, and then the resulting residue was applied to a silica gel column chromatography to obtain 0.16 g of 6-(2-ethylsulfanylphenyl)-5-methyl-2-trifluoromethylimidazo[1,2-a]pyridine (Compound of Present Invention 28).

WORKUP

后处理

  1. temperatureunder heat-reflux for 3 hours
  2. stirringthe mixture was stirred
  3. temperatureunder heat-reflux for 5 hours
  4. filtrationthe mixture was filtered
  5. extractionThe filtrate was extracted with ethyl acetate
  6. dry with materialdried over anhydrous sodium sulfate
  7. concentrationThe dried matter was concentrated under reduced pressure