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To an ice cooled stirred solution of 3-nitro-5-(trifluoromethyl)benzoic acid (25.00 g, 106.3 mmol) in methanol (500 mL) was added acetyl chloride (22.00 g, 280.2 mmol) dropwise over 20 min. After the addition was complete, the reaction mixture was stirred for 20 min at 0° C., then heated at reflux for 6 h and then cooled to room temperature. The reaction mixture was concentrated under reduced pressure and the residue was dissolved in ethyl acetate, washed with saturated aqueous sodium bicarbonate, filtered through a silica gel and concentrated under reduced pressure to provide methyl 3-nitro-5-(trifluoromethyl)benzoate (24.65 g, 93%) as a pale yellow oil.

1. additionAfter the addition
2. temperatureheated
3. temperatureat reflux for 6 h
4. temperaturecooled to room temperature
5. concentrationThe reaction mixture was concentrated under reduced pressure
6. dissolutionthe residue was dissolved in ethyl acetate
7. washwashed with saturated aqueous sodium bicarbonate
8. filtrationfiltered through a silica gel
9. concentrationconcentrated under reduced pressure