HRID570724

反应详情

EQUATION

反应方程式

HRID 570724 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-(Ethylsulfanyl)-7-(hydroxymethyl)-3-[4-(2,2,2-trifluoroethoxy)phenyl]pyrido[2,3-d]pyrimidin-4(3H)-one (373 mg) and triethylamine (6 ml) were dissolved in dimethyl sulfoxide (18 ml), sulfur trioxide pyridine complex (1.16 g) was added thereto by several portions, and the mixture was stirred at room temperature for 1 hr. To the reaction mixture was added water, and the mixture was extracted with ethyl acetate. The extract was washed with water, 1M hydrochloric acid and saturated brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give the title compound (299 mg) as a orange solid.

WORKUP

后处理

  1. additionsulfur trioxide pyridine complex (1.16 g) was added
  2. extractionthe mixture was extracted with ethyl acetate
  3. washThe extract was washed with water, 1M hydrochloric acid and saturated brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe obtained residue was purified by silica gel column chromatography (ethyl acetate/hexane)