반응 #312480

반응 방정식

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

반응 조건

후처리

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

실험 절차

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.

출처