Reaktionsgleichung
[F:1][C:2]([F:22])([F:21])[C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([C:9]2[N:14]3[N:15]=[CH:16][C:17]([C:18]([NH2:20])=O)=[C:13]3[N:12]=[CH:11][CH:10]=2)[CH:4]=1.P(Cl)(Cl)(Cl)=O>>[F:21][C:2]([F:1])([F:22])[C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([C:9]2[N:14]3[N:15]=[CH:16][C:17]([C:18]#[N:20])=[C:13]3[N:12]=[CH:11][CH:10]=2)[CH:4]=1Komponenten
3
Versuchsvorschrift
One gram of 7-(α,α,α-trifluoro-m-tolyl)pyrazolo[1,5-a]pyrimidine-3-carboxamide and 5 ml. of phosphorus oxychloride is refluxed for 3 hours. The reaction mixture is evaporated to dryness and the residue is dissolved in methylene chloride, washed with saturated sodium bicarbonate solution, dried with anhydrous sodium sulfate. After passing through a short pad of hydrous magnesium silicate with eluent methylene chloride. Concentration of the eluent with addition of n-hexane gives the product, m.p. 141°-143° C.
Aufarbeitung
- customThe reaction mixture is evaporated to dryness
- dissolutionthe residue is dissolved in methylene chloride
- washwashed with saturated sodium bicarbonate solution
- dry with materialdried with anhydrous sodium sulfate
- additionConcentration of the eluent with addition of n-hexane
- customgives the product, m.p. 141°-143° C.
Quellen und Nachweise
- ORD-Eintrag
- ord-67ede502dbfe46ea9f2258b8197708ba
- Quelldatensatz
- uspto-grants-1979_12
- Patentnummer
- US04178449
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