Reaktionsgleichung
[F:1][C:2]([F:22])([F:21])[C:3]1[CH:4]=[C:5]([C:9]2[N:14]3[N:15]=[CH:16][C:17]([C:18]([NH2:20])=[O:19])=[C:13]3[NH:12][CH2:11][CH:10]=2)[CH:6]=[CH:7][CH:8]=1.C([SiH](CC)CC)C.[OH-].[K+]>FC(F)(F)C(O)=O>[F:21][C:2]([F:1])([F:22])[C:3]1[CH:4]=[C:5]([CH:9]2[N:14]3[N:15]=[CH:16][C:17]([C:18]([NH2:20])=[O:19])=[C:13]3[NH:12][CH2:11][CH2:10]2)[CH:6]=[CH:7][CH:8]=1Komponenten
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 60 °C
Versuchsvorschrift
A solution of 3.44 g of 4,5-dihydro-7-[3-(trifluoromethyl)phenyl]pyrazolo[1,5-a]pyrimidine-3-carboxamide (Ex. 24) in 40 ml of trifluoroacetic acid was stirred under nitrogen and heated to 60° C. in an oil bath. Then 5.0 ml of triethylsilane was added and the mixture was stirred at 60° C. for 24 hours. The reaction mixture was cooled and carefully poured into a beaker containing a 25% aqueous solution of potassium hydroxide and cracked ice. The product which precipitated was extracted into chloroform. The chloroform was washed with water, dried over anhydrous sodium sulfate and filtered. The filtrate was evaporated in vacuo and gave crystals which were recrystallized from toluene-hexane to give the desired product, mp 152°-154° C.
Aufarbeitung
- temperatureThe reaction mixture was cooled
- additioncarefully poured into a beaker
- customThe product which precipitated
- extractionwas extracted into chloroform
- washThe chloroform was washed with water
- dry with materialdried over anhydrous sodium sulfate
- filtrationfiltered
- customThe filtrate was evaporated in vacuo
- customgave crystals which
- customwere recrystallized from toluene-hexane
Quellen und Nachweise
- ORD-Eintrag
- ord-eec79a0350064775b60e18124d16bc30
- Quelldatensatz
- uspto-grants-1989_07
- Patentnummer
- US04847256
Verknüpfte Notizen
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