反应详情

温度

140 °C

4-Amino-2,3-difluoro-5-nitro-benzoic acid methyl ester 4 (2.00 g, 8.62 mmol) is suspended in xylenes (15 mL) and 2-chloro aniline (9.06 mL, 86.15 mmol) is added. The reaction mixture is heated to 140° C. under a nitrogen atmosphere. After 6 days, the reaction mixture is cooled to room temperature, and diluted with ethyl acetate. The reaction mixture is washed with water, 10% HCl solution and brine. The organic layer is dried (MgSO4) and concentrated under reduced pressure. The crude product is triturated with diethyl ether, twice, to give 0.35 g (12%) pure desired product as a brownish solid.

1. temperaturethe reaction mixture is cooled to room temperature
2. washThe reaction mixture is washed with water, 10% HCl solution and brine
3. dry with materialThe organic layer is dried (MgSO4)
4. concentrationconcentrated under reduced pressure
5. customThe crude product is triturated with diethyl ether