Reaktionsgleichung
[Cl:1][C:2]1[CH:3]=[C:4]([S:9][C:10]2[N:14](CC3C=CC(OC)=CC=3)[N:13]=[C:12]([CH3:24])[C:11]=2[C:25]([C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=2)=[O:26])[CH:5]=[C:6]([Cl:8])[CH:7]=1.FC(F)(F)C(O)=O>>[Cl:8][C:6]1[CH:5]=[C:4]([S:9][C:10]2[NH:14][N:13]=[C:12]([CH3:24])[C:11]=2[C:25]([C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=2)=[O:26])[CH:3]=[C:2]([Cl:1])[CH:7]=1Komponenten
3
Versuchsvorschrift
140 mg of [5-(3,5-dichlorophenylthio)-1-(4-methoxybenzyl)-3-methyl-1H-pyrazol-4-yl]-phenyl-methanone was treated with 4 ml of trifluoroacetic acid. The solution was then heated at reflux for 2 h. The solvent was evaporated under reduced pressure. The residue was then partitioned between dichloromethane/saturated sodium hydrogen carbonate, washed with brine then dried over anhydrous magnesium sulphate, filtered and evaporated to give 75 mg of [5-(3,5-dichlorophenylthio)-3-methyl-1H-pyrazol-4-yl]-phenyl-methanone as a yellow solid which was used without further purification. Mass spectrum (ES) m/z 363[M+H]+.
Aufarbeitung
- temperatureThe solution was then heated
- temperatureat reflux for 2 h
- customThe solvent was evaporated under reduced pressure
- customThe residue was then partitioned between dichloromethane/saturated sodium hydrogen carbonate
- washwashed with brine
- dry with materialthen dried over anhydrous magnesium sulphate
- filtrationfiltered
- customevaporated
Quellen und Nachweise
- ORD-Eintrag
- ord-e9eeffe890ec4d609dcb2396330d5e76
- Quelldatensatz
- uspto-grants-2004_03
- Patentnummer
- US06699887B2
Verknüpfte Notizen
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