HRID1940910

反应详情

EQUATION

反应方程式

HRID 1940910 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-Benzylthio-5,8-dichloro[1,2,4]triazolo[1,5-a]pyridine (6.0 g, 0.019 mol) and 25 percent sodium methoxide in methanol (26.5 mL, 6.3 g, 0.116 mol) were combined in methanol and the mixture was heated to reflux for 2 hours. The mixture was then cooled, acidified with acetic acid, and concentrated by evaporation under reduced pressure. The residue was dissolved in dichloromethane and the solution was washed with water and concentrated by evaporation under reduced pressure. The residue was triturated with hexane and the resulting solids were collected by filtration and dried to obtain 5.76 g (99 percent of theory) of the title compound as a light tan powder melting at 90°-91° C.

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureto reflux for 2 hours
  3. temperatureThe mixture was then cooled
  4. concentrationconcentrated by evaporation under reduced pressure
  5. dissolutionThe residue was dissolved in dichloromethane
  6. washthe solution was washed with water
  7. concentrationconcentrated by evaporation under reduced pressure
  8. customThe residue was triturated with hexane
  9. filtrationthe resulting solids were collected by filtration
  10. customdried