Reaktionsgleichung
[CH3:1][C:2]([C:4]1[CH:9]=[CH:8][C:7]([C:10]([F:13])([F:12])[F:11])=[CH:6][CH:5]=1)=[O:3].C(O)C.[H-].[Na+].Cl.[C:20](=O)([O-:24])[O:21][CH2:22][CH3:23]>O>[O:3]=[C:2]([C:4]1[CH:9]=[CH:8][C:7]([C:10]([F:11])([F:12])[F:13])=[CH:6][CH:5]=1)[CH2:1][C:20]([O:21][CH2:22][CH3:23])=[O:24]Komponenten
Versuchsvorschrift
To a solution of 4-trifluoromethylacetophenone (57.8 g, 0.307 mol) and ethanol (1 ml) in ethyl carbonate (300 ml) was added sodium hydride (24.5 g, 60% in oil, 0.63 mol) by small portions. Because heat was generated gradually, the reaction solution was ice-cooled and thereafter stirred at room temperature for 2 hrs. 6N Hydrochloric acid was added thereto to stop the reaction. The mixture was diluted with water (300 ml) and extracted with ethyl acetate (200 ml×2). The extract was washed with water, dried over anhydrous magnesium sulfate and evaporated under reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=50:1-5:1) to give ethyl 3-oxo-3-(4-trifluoromethylphenyl)propionate (71.2 g, 89%).
Aufarbeitung
- temperatureBecause heat
- temperaturecooled
- customthe reaction
- extractionextracted with ethyl acetate (200 ml×2)
- washThe extract was washed with water
- dry with materialdried over anhydrous magnesium sulfate
- customevaporated under reduced pressure
- customThe residue was purified by silica gel column chromatography (hexane:ethyl acetate=50:1-5:1)
Quellen und Nachweise
- ORD-Eintrag
- ord-57f7af035cca4cbfb9ed65a90717848e
- Quelldatensatz
- uspto-grants-2006_01
- Patentnummer
- US06982348B2
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