Реакция #91063

Уравнение реакции

4-chlor-3-(trifluoromethyl)benzoic acid

sulfuric acid

methanol

→

title compound

Methyl 4-Chloro-3-(trifluoromethyl)benzoate

Условия реакции

Обработка

1. 1
   ТемператураThe mixture was heated
2. 2
   Температураunder reflux overnight
3. 3
   Концентрированиеconcentrated under reduced pressure
4. 4
   Другоеto form a solid
5. 5
   ФильтрацияThe solid was filtered
6. 6
   Промывкаwashed with water
7. 7
   Другоеto remove any residual sulfuric acid
8. 8
   Фильтрацияfiltered
9. 9
   Другоеdried under vacuum

Методика

To a solution of 4-chlor-3-(trifluoromethyl)benzoic acid (1037 g, 46.2 mmol) in methanol (100 mL) was added concentrated sulfuric acid (0.51 mL, 9.24 mmol). The mixture was heated under reflux overnight. The mixture was allowed to cool to room temperature and concentrated under reduced pressure to form a solid. The solid was filtered and washed with water. The solid was then stirred with saturated aqueous sodium bicarbonate solution to remove any residual sulfuric acid, filtered and dried under vacuum to give the title compound as a white solid (10.18 g). 1H NMR (400 MHz, CDCl3) δ ppm 3.96 (s, 31), 7.60 (d, J=8.34 Hz, 1H), 8.14 (dd, J=8.34, 2.02 Hz, 1H), 8.37 (d, J 2.02 Hz, 1H).

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