反应 #302897

反应方程式

sulfuric acid

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

methanol

→

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

反应条件

后处理

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
   其他the solvent was removed
5. 5
   萃取the mixture was extracted twice with ethyl acetate
6. 6
   洗涤The combined organic phases were washed once with saturated aqueous NaHCO3 solution
7. 7
   其他Finally, the organic phase was dried
8. 8
   浓缩the filtrate was concentrated

实验过程

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.

来源