反应 #312480

反应方程式

NaOH

phosphorus

dimethylformamide

7-(α,α,α-trifluoro-m-tolyl)pyrazolo[1,5-a]pyrimidine

→

7-(α,α,α-Trifluoro-m-tolyl)pyrazolo[1,5-a]pyrimidine-3-carboxaldehyde

反应条件

后处理

1. 1
   workup.ADDITIONThe mixture is poured onto ice
2. 2
   其他The precipitated solid is removed by filtration
3. 3
   其他recrystallized from methylene chloride-hexane
4. 4
   其他to give the product, m.p. 196°-198° C.

实验过程

Seventy-five milliliters of dried dimethylformamide is cooled in an ice bath and 25 ml. of phosphorus osychloride is added dropwise with swirling. To this ice cold mixture is added 19.5 g. of 7-(α,α,α-trifluoro-m-tolyl)pyrazolo[1,5-a]pyrimidine in one portion and the reaction mixture is then heated on a steam bath for 1.5 hours. The mixture is poured onto ice and made basic (pH 10) with 10 N NaOH. The precipitated solid is removed by filtration and recrystallized from methylene chloride-hexane to give the product, m.p. 196°-198° C.

来源