Hydrochloric Acid → HCID 59556306, Verbindung
Reaktionsgleichung
[CH3:1][C:2]1[N:3]=[C:4]([C:9]2[CH:14]=[CH:13][C:12]([C:15]([F:18])([F:17])[F:16])=[CH:11][CH:10]=2)[S:5][C:6]=1[CH:7]=[O:8].Br[C:20]([F:24])([F:23])[CH:21]=[CH2:22].Cl>CN(C)C=O>[F:23][C:20]([F:24])([CH:21]=[CH2:22])[CH:7]([C:6]1[S:5][C:4]([C:9]2[CH:10]=[CH:11][C:12]([C:15]([F:18])([F:16])[F:17])=[CH:13][CH:14]=2)=[N:3][C:2]=1[CH3:1])[OH:8]Komponenten
5
Versuchsvorschrift
To a solution of 1.0 g 4-Methyl-2-(4-trifluoromethyl-phenyl)-thiazole-5-carbaldehyde and 868 mg 3-bromo-3,3-difluorpropene in 10 ml dimethylformamide 425 mg Indium were added and the resulting suspension was stirred in an ultrasonic bath for two hours. Then 20 ml 1 N hydrochloric acid were added and the mixture stirred at room temperature for thirty minutes. The mixture was extracted three times with portions of 50 ml ethyl acetate. The combined organic layers were dried over MgSO4. The solvent was evaporated in vacuo. The resulting residue was purified by reversed phase HPLC to obtain 740 mg 2,2-Difluoro-1-[4-methyl-2-(4-trifluoromethyl-phenyl)-thiazol-5-yl]-but-3-en-1-ol as a colorless lyophilisate.
Aufarbeitung
- stirringthe mixture stirred at room temperature for thirty minutes
- extractionThe mixture was extracted three times with portions of 50 ml ethyl acetate
- dry with materialThe combined organic layers were dried over MgSO4
- customThe solvent was evaporated in vacuo
- customThe resulting residue was purified by reversed phase HPLC
Quellen und Nachweise
- ORD-Eintrag
- ord-51237ab247af471281c0608f9fa68260
- Quelldatensatz
- uspto-grants-2010_11
- Patentnummer
- US07834030B2
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