Reaktionsgleichung
Cl[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]([F:11])([F:10])[F:9].[C:12](=O)([O-:14])[O-:13].[Na+].[Na+].[C]=O>[Pd](Cl)Cl.C1(P(C(C(P(C2C=CC=CC=2)C2C=CC=CC=2)C)C)C2C=CC=CC=2)C=CC=CC=1.O>[F:9][C:8]([F:11])([F:10])[C:3]1[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=1[C:12]([OH:14])=[O:13]Komponenten
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 3
Reaktionsbedingungen
- Temperatur
- 210 °C
Versuchsvorschrift
In an autoclave made of metal were placed 18 g of ortho-chlorobenzotrifluoride, 3.5 mg of palladium chloride, 170 mg of bisdiphenylphosphinobutane and 23 g of sodium carbonate. The air in the autoclave was replaced with carbon monoxide introduced thereinto in several times, after which carbon monoxide was further introduced to adjust its pressure therein to 30 kg/cm2. The reaction was carried out with stirring for 5 hours on a salt bath at a bath temperature of 210° C. After completion of the reaction, the reaction mixture was cooled to room temperature and water was added. The aqueous layer was separated and then acid was added thereto, followed by extraction from the aqueous layer with ether. The ether layer was dried and then concentrated to obtain 2.8 g of ortho-trifluoromethylbenzoic acid.
Aufarbeitung
- additionintroduced
- customAfter completion of the reaction
- temperaturethe reaction mixture was cooled to room temperature
- customThe aqueous layer was separated
- additionacid was added
- extractionfollowed by extraction from the aqueous layer with ether
- dry with materialThe ether layer was dried
- concentrationconcentrated
Quellen und Nachweise
- ORD-Eintrag
- ord-1c4f0af3f1144aa298d604a1e633c720
- Quelldatensatz
- uspto-grants-1993_03
- Patentnummer
- US05194631
Verknüpfte Notizen
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