反应详情

温度

140 °C

To 304.35 g of 4-carboxymethyl-3,5,6-trifluorophthalic acid dissolved in 1.5 liters of dimethyl sulfoxide was added 0.5 liter of triethylamine, followed by 64 hours of stirring at 140° C. After cooling to room temperature, dimethyl sulfoxide was evaporated. The resulting residue was mixed with 1 liter of 1N hydrochloric acid and extracted with ether (1 liter×3). The organic layer was washed with 1 liter of water and 1 liter of saturated brine, and then dried over sodium sulfate. By evaporating the solvent, 177.94 g (0.64 mol, 60%) of the title compound was obtained as a partially purified product.

1. temperatureAfter cooling to room temperature
2. customdimethyl sulfoxide was evaporated
3. additionThe resulting residue was mixed with 1 liter of 1N hydrochloric acid
4. extractionextracted with ether (1 liter×3)
5. washThe organic layer was washed with 1 liter of water and 1 liter of saturated brine
6. dry with materialdried over sodium sulfate
7. customBy evaporating the solvent