反应详情

Bis(2-chloro-4-fluoro-5-nitrophenyl)carbonate (1.2 Kg, 2.9 mol), toluene (7 liters) as a solvent and 5% Pd/C (200 g) as a catalyst were placed in a 10L three-necked flask equipped with a stirrer, and hydrogen gas was introduced while vigorously stirring. Heat generated as the reaction proceeded, and the reaction temperature was maintained at 60° to 70° C. by introducing hydrogen at such a rate that the hydrogen gas did not discharge from the system. After completion of the reaction, the reaction mixture was heated (60°-70° C.), and the catalyst was separated by filtration. The organic layer of the filtrate was separated and dried over anhydrous magnesium sulfate. The drying agent was separated by filtration, and the solvent was distilled off under reduced pressure to obtain bis(2-chloro-4-fluoro-5-aminophenyl)carbonate as a white solid (1.01Kg, 2.89 mol, 99.6% yield).

1. customequipped with a stirrer
2. temperatureHeat
3. temperaturethe reaction temperature was maintained at 60° to 70° C.
4. customAfter completion of the reaction
5. temperaturethe reaction mixture was heated (60°-70° C.)
6. customthe catalyst was separated by filtration
7. customThe organic layer of the filtrate was separated
8. dry with materialdried over anhydrous magnesium sulfate
9. customThe drying agent was separated by filtration
10. distillationthe solvent was distilled off under reduced pressure