HRID963161
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturethe mixture was heated
- temperatureto reflux for 2 hours
- temperatureThe mixture was then cooled
- concentrationconcentrated by evaporation under reduced pressure
- dissolutionThe residue was dissolved in dichloromethane
- washthe solution was washed with water
- concentrationconcentrated by evaporation under reduced pressure The residue
- customwas triturated with hexane
- filtrationthe resulting solids were collected by filtration
- customdried