反应详情

A 3.3 g. portion of N-chlorobenzotriazole is added to a solution of 5.26 g. of 7-(α,α,α-trifluoro-m-tolyl)pyrazolo[1,5-a]pyrimidine in 50 ml. of chloroform producing an exothermic reaction. The mixture is refluxed on a steam bath for 15 minutes, cooled to room temperature and then poured into an ice-cold solution of 2.5 N sodium hydroxide. The organic layer is separated, dried over socium sulfate and passed through a hydrous magnesium silicate column. The effluent is heated to reflux and hexane is added giving a solid. The solid is dissolved in methylene chloride re-processed through the column and precipitated from refluxing solution with hexane giving crystals of the desired product, m.p. 155°-157° C.

1. temperatureThe mixture is refluxed on a steam bath for 15 minutes
2. customThe organic layer is separated
3. dry with materialdried over socium sulfate
4. temperatureThe effluent is heated
5. temperatureto reflux
6. additionhexane is added
7. customgiving a solid
8. customprecipitated
9. temperaturefrom refluxing solution with hexane giving crystals of the desired product, m.p. 155°-157° C.