Reaktionsgleichung
C([O:4][C:5](=[O:22])[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[C:12]1[CH:17]=[CH:16][C:15]([C:18]([F:21])([F:20])[F:19])=[CH:14][N:13]=1)(C)C.O.[OH-].[Li+]>O1CCCC1CO.O>[F:20][C:18]([F:19])([F:21])[C:15]1[CH:16]=[CH:17][C:12]([C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=2[C:5]([OH:22])=[O:4])=[N:13][CH:14]=1Komponenten
4
Versuchsvorschrift
2-(5-Trifluoromethyl-pyridin-2-yl)-benzoic acid isopropyl ester was dissolved in 10 ml of a 3:1:1 mixture of tetrahydrofuran-methanol-water, and lithium hydroxide monohydrate (161 mg, 3.84 mmol) was added. After stirring for 3 h at room temperature, the volatiles were removed under vacuum and 5 ml of water were added to the mixture, which was brought to pH 6 with 1N HCl. The resulting slurry was extracted with ethyl acetate, the combined organic layers were dried (magnesium sulfate), filtered and concentrated under vacuum to provide the title compound.
Aufarbeitung
- additionwas added
- customthe volatiles were removed under vacuum and 5 ml of water
- additionwere added to the mixture, which
- extractionThe resulting slurry was extracted with ethyl acetate
- dry with materialthe combined organic layers were dried (magnesium sulfate)
- filtrationfiltered
- concentrationconcentrated under vacuum
Quellen und Nachweise
- ORD-Eintrag
- ord-ba7b74c984b54a368ce98a401e2c202e
- Quelldatensatz
- uspto-grants-2002_04
- Patentnummer
- US06369075B1
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