Reaktionsgleichung
[F:1][C:2]([F:17])([F:16])[C:3]1[CH:4]=[C:5]([NH:9]C2C=CC=CC=2)[CH:6]=[CH:7][CH:8]=1.[C:18]([OH:22])(=[O:21])[CH:19]=[CH2:20].[OH-].[Na+]>O>[F:1][C:2]([F:16])([F:17])[C:3]1[CH:4]=[C:5]([NH:9][CH2:20][CH2:19][C:18]([OH:22])=[O:21])[CH:6]=[CH:7][CH:8]=1Komponenten
5
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 100 °C
Versuchsvorschrift
To an aqueous solution of 3-trifluoromethylphenyl aniline (5.0 g) in water (15.0 ml) was added acrylic acid (3.2 ml) and the resulting mixture was stirred at 100° C. for one hour. The reaction mixture was basified with 5N aqueous sodium hydroxide solution and extracted with ethyl acetate (100 ml×2). The resulting organic layer was washed with saturated saline (50 ml), dried over anhydrous sodium sulfate and then concentrated under reduced pressure. The residue was purified by silica gel column chromatography (eluent: chloroform/methanol) to afford 3-(3-trifluoromethylphenylamino)propionic acid (8.4 g).
Aufarbeitung
- extractionextracted with ethyl acetate (100 ml×2)
- washThe resulting organic layer was washed with saturated saline (50 ml)
- dry with materialdried over anhydrous sodium sulfate
- concentrationconcentrated under reduced pressure
- customThe residue was purified by silica gel column chromatography (eluent: chloroform/methanol)
Quellen und Nachweise
- ORD-Eintrag
- ord-26b75629e775465c8819f182137e5e1b
- Quelldatensatz
- uspto-grants-2015_05
- Patentnummer
- US09040516B2
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