反应详情

N-benzyloxy-2-(2,4-difluoroanilino)-4,5-difluoro-benzamide (Example I-4, 5.66 g, 15 mmol) and carbonyldiimidazole (2.83 g, 17 mmol) were combined in 300 mL of THF and heated to reflux for 30 hours. The solution was cooled, concentrated, and redissolved in chloroform. The solution was washed with 1N HCl, saturated NaHCO3, brine, and dried over magnesium sulfate. The solution was concentrated to give 4.25 g of a solid which was purified by column chromatography (silica gel, CHCl3/MeOH, 98:2) to give 2.0 g of the title compound as a solid.

1. temperatureheated
2. temperatureto reflux for 30 hours
3. temperatureThe solution was cooled
4. concentrationconcentrated
5. dissolutionredissolved in chloroform
6. washThe solution was washed with 1N HCl, saturated NaHCO3, brine
7. dry with materialdried over magnesium sulfate
8. concentrationThe solution was concentrated