Reaktionsgleichung
C([O:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=1[O:16][CH2:17][CH2:18][CH2:19][NH:20][C:21](=[O:32])[C:22]1[CH:27]=[CH:26][C:25]([C:28]([F:31])([F:30])[F:29])=[CH:24][CH:23]=1)(=O)C1C=CC=CC=1.CO.[OH-].[Na+].Cl>O>[F:29][C:28]([F:30])([F:31])[C:25]1[CH:26]=[CH:27][C:22]([C:21]([NH:20][CH2:19][CH2:18][CH2:17][O:16][C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=2[OH:9])=[O:32])=[CH:23][CH:24]=1Komponenten
6
Reaktionsbedingungen
- Temperatur
- 0 °C
Versuchsvorschrift
To a mixture of 0.87 g of 3-ethyl-5-methyl-4-(3-(4-(trifluoromethyl)benzamido)propyloxyphenyl benzoate and 10 ml of methanol was added a mixture of 0.16 g of sodium hydroxide and 2 m of water, while stirring at 0° C. After stirring at room temperature for 24 hours, the reaction mixture was made weak acidic by the addition of 10% hydrochloric acid, and extracted with 50 ml of ethyl acetate. The ethyl acetate layer was washed with saturated saline solution, dried over anhydrous magnesium sulfate, and then concentrated under reduced pressure to give a residue. The residue was subjected to silica gel chromatography, which afforded 0.66 g of 3-ethyl-5-methyl-4-(3-(4-(trifluoromethyl)benzamido)propyloxyphenol (94% yield).
Aufarbeitung
- additionwas added
- stirringAfter stirring at room temperature for 24 hours
- extractionextracted with 50 ml of ethyl acetate
- washThe ethyl acetate layer was washed with saturated saline solution
- dry with materialdried over anhydrous magnesium sulfate
- concentrationconcentrated under reduced pressure
- customto give a residue
Quellen und Nachweise
- ORD-Eintrag
- ord-cdf1e3aa33c043e3ade040d9bac596ec
- Quelldatensatz
- uspto-grants-2001_04
- Patentnummer
- US06214835B1
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