HRID963152

反应详情

EQUATION

反应方程式

HRID 963152 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 2-benzylthio-5-chloro-7-methyl[1,2,4]triazolo[1,5-a]pyridine (5.0 g, 0.017 mol), sodium methoxide in methanol (16 mL of 25 percent, 3.7 g, 0.070 mol) and methanol (100 mL) were heated at reflux with stirring for 4 hours. The reaction mixture was then cooled, acidified with acetic acid (10 mL), and concentrated by evaporation under reduced pressure. The residue obtained was dissolved in dichloromethane and the resulting solution was washed well with water, dried over magnesium sulfate, and concentrated by evaporation under reduced pressure. The residue obtained was mixed with hexane and filtered to recover the solids. The solids were dried to obtain 4.7 g (97 percent of theory) of the title compound as a tan powder melting at 85°-87° C.

WORKUP

后处理

  1. temperaturewere heated
  2. temperatureat reflux
  3. temperatureThe reaction mixture was then cooled
  4. concentrationconcentrated by evaporation under reduced pressure
  5. customThe residue obtained
  6. washthe resulting solution was washed well with water
  7. dry with materialdried over magnesium sulfate
  8. concentrationconcentrated by evaporation under reduced pressure
  9. customThe residue obtained
  10. filtrationfiltered
  11. customto recover the solids
  12. customThe solids were dried