反応 #302897

反応方程式

sulfuric acid

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

methanol

→

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

反応条件

後処理

1. 1
   温度the mixture was heated
2. 2
   温度under reflux until HPLC analysis
3. 3
   温度The mixture was cooled
4. 4
   その他the solvent was removed
5. 5
   抽出the mixture was extracted twice with ethyl acetate
6. 6
   洗浄The combined organic phases were washed once with saturated aqueous NaHCO3 solution
7. 7
   その他Finally, the organic phase was dried
8. 8
   濃縮the filtrate was concentrated

実験手順

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.

出典