Реакция #302897

Уравнение реакции

sulfuric acid

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

methanol

→

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

Условия реакции

Обработка

1. 1
   Температураthe mixture was heated
2. 2
   Температураunder reflux until HPLC analysis
3. 3
   ТемператураThe mixture was cooled
4. 4
   Другоеthe solvent was removed
5. 5
   Экстракцияthe mixture was extracted twice with ethyl acetate
6. 6
   ПромывкаThe combined organic phases were washed once with saturated aqueous NaHCO3 solution
7. 7
   ДругоеFinally, the organic phase was dried
8. 8
   Концентрированиеthe filtrate was concentrated

Методика

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.

Источник