HRID1851161

反应详情

EQUATION

反应方程式

HRID 1851161 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

2.35 g (7.5 mmol) 5,7-Dichloro-6-(2,4-difluorophenyl)-2-methyl-[1,2,4]triazolo[1,5-a]pyrimidine are given in 189 mL ethanol, 135 mL water and 73 mL THF. 1.89 g (35.3 mmol) NH4Cl and 3.1 g (47.7 mmol) zinc powder are added and the mixture is stirred at room temperature for 3 h. The reaction mixture is filtered and the organic solvents are removed. The residue is diluted with water and extracted three times with ethyl acetate. The combined organic layers are washed with brine and dried over Na2SO4. After evaporation of the solvent, the residue is purified by chromatography. 1.2 g (51.6%) of the desired product are obtained.

WORKUP

后处理

  1. filtrationThe reaction mixture is filtered
  2. customthe organic solvents are removed
  3. additionThe residue is diluted with water
  4. extractionextracted three times with ethyl acetate
  5. washThe combined organic layers are washed with brine
  6. dry with materialdried over Na2SO4
  7. customAfter evaporation of the solvent
  8. customthe residue is purified by chromatography