HRID1775276

反应详情

EQUATION

反应方程式

HRID 1775276 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A mixture of 156 mg of 1-[2-(2-ethylsulfanylphenyl)-7-trifluoromethylpyrido[3,2-d]pyrimidin-4-yl]-2-tosylhydrazine and 12 ml of ethylene glycol was added to a mixture of 4 ml of an 8% aqueous sodium hydroxide solution and 2 ml of ethylene glycol at 80° C., and the mixture was stirred at 100° C. for 40 minutes. Water was added to the cooled reaction mixture, and the mixture was extracted with t-butyl methyl ether. The organic layer was washed with water, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The mixture was concentrated under reduced pressure, and the resulting residue was applied to a silica gel column chromatography to obtain 40 mg of 2-(2-ethylsulfanylphenyl)-7-trifluoromethylpyrido[3,2-d]pyrimidine (Compound of Present Invention 18).

WORKUP

后处理

  1. extractionthe mixture was extracted with t-butyl methyl ether
  2. washThe organic layer was washed with water
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. concentrationThe mixture was concentrated under reduced pressure