Carbon Dioxide → 4-Chloro-2-(trifluoromethyl)benzoic acid
Reaktionsgleichung
[Cl:1][C:2]1[CH:7]=[CH:6][C:5](I)=[C:4]([C:9]([F:12])([F:11])[F:10])[CH:3]=1.[Mg].[C:14](=[O:16])=[O:15].Cl>CCOCC>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:14]([OH:16])=[O:15])=[C:4]([C:9]([F:12])([F:11])[F:10])[CH:3]=1Komponenten
Edukt 4
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 0 °C
Versuchsvorschrift
A solution of 4-chloro-2-trifluoromethyliodobenzene (100 g) in ether was added to a suspension of magnesium (8 g) in ether at a such a rate as to maintain the mixture at reflux. The mixture was stirred at reflux for 1 hour and then cooled to 0° C. Carbon dioxide was then passed into the stirred mixture for 3 hours. Hydrochloric acid (2M) was added and the resulting layers separated. The organic layer was washed with water and then extracted into aqueous sodium carbonate solution and this aqueous extract was acidified to pH 1 and extracted with ether. The ether layer was washed with saturated sodium chloride solution, dried (anhydrous magnesium sulphate) and the solvent evaporated to give 4-chloro-2-trifluoromethylbenzoic acid (57.1 g) as a brown solid, m.p. 106.5°-108° C.
Aufarbeitung
- temperatureto maintain the mixture
- temperatureat reflux
- temperatureat reflux for 1 hour
- customthe resulting layers separated
- washThe organic layer was washed with water
- extractionextracted into aqueous sodium carbonate solution
- extractionthis aqueous extract
- extractionextracted with ether
- washThe ether layer was washed with saturated sodium chloride solution
- dry with materialdried (anhydrous magnesium sulphate)
- customthe solvent evaporated
Quellen und Nachweise
- ORD-Eintrag
- ord-43e5e965975f48cbb98b599a387aef85
- Quelldatensatz
- uspto-grants-1997_07
- Patentnummer
- US05650533
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