Reaktion #302897

Reaktionsgleichung

sulfuric acid

2-fluoro-3-methylthio-4-(trifluoromethyl)benzoic acid

methanol

→

methyl 2-fluoro-3-methylthio-4-(trifluoromethyl)benzoate

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturthe mixture was heated
2. 2
   Temperaturunder reflux until HPLC analysis
3. 3
   TemperaturThe mixture was cooled
4. 4
   Sonstigethe solvent was removed
5. 5
   Extraktionthe mixture was extracted twice with ethyl acetate
6. 6
   WaschenThe combined organic phases were washed once with saturated aqueous NaHCO3 solution
7. 7
   SonstigeFinally, the organic phase was dried
8. 8
   Einengenthe filtrate was concentrated

Vorschrift

5 ml of concentrated sulfuric acid were added to 20.0 g (78.7 mmol) of 2-fluoro-3-methylthio-4-(trifluoromethyl)benzoic acid in 200 ml of methanol, and the mixture was heated under reflux until HPLC analysis showed complete conversion. The mixture was cooled and the solvent was removed. The residue was taken up in water, and the mixture was extracted twice with ethyl acetate. The combined organic phases were washed once with saturated aqueous NaHCO3 solution. Finally, the organic phase was dried and the filtrate was concentrated. This gave 20.5 g of methyl 2-fluoro-3-methylthio-4-(trifluoromethyl)benzoate.

Quelle