反应详情

温度

195 °C

2-amino-5-bromophenol (1.72 g, 9.2 mmol) and 2-fluoro-4-(methylsulfonyl)benzoic acid (2 g, 9.2 mmol) were dissolved in polyposphoric acid (30 g). This mixture was heated at 195° C. for three and half hours. Reaction mixture cooled to rt and diluted with ice water (100 ml). Aqueous layer basified with sodium hydroxide pellets to pH 9. Solid that formed was filtered and dried to obtain the crude. Crude was purified by combiflash using a gradient mixture of EtOAc and Petether (1:3) as eluent to afford the titled compound (450 mg) as a dark brown solid.

1. customReaction mixture
2. temperaturecooled to rt
3. customSolid that formed
4. filtrationwas filtered
5. customdried
6. customto obtain the crude
7. customCrude was purified by combiflash
8. additiona gradient mixture of EtOAc and Petether (1:3) as eluent