反应详情

温度

95 °C

To a reactor was added 24 g of 3-chloro-2-(diphenylmethyleneamino) pyridin-4(1H)-one, DMF (100 mL), cesium carbonate (12.7 g; 0.5 eq) and difluoronitrobenzene (9.3 mL; 1.1 eq). The reaction mixture was heated to 95° C. and stirred for three hours. After the reaction was complete, the reaction mixture was poured onto crushed ice and the solids were filtered off and washed with water. The crude solids were charged back to the reactor and dissolved in THF (200 mL). Methanol was added and the mixture was distilled at a constant volume of 350 mL, until THF had been azeotropically removed. Additional methanol (100 mL) was added and the suspension was cooled to room temperature. The solids were filtered and dried under vacuum to yield 3-Chloro-N-(diphenylmethylene)-4-(2-fluoro-4-nitrophenoxy) pyridin-2-amine (23.3 g; 67% yield).

1. additionthe reaction mixture was poured
2. customonto crushed ice
3. filtrationthe solids were filtered off
4. washwashed with water
5. additionThe crude solids were charged back to the reactor
6. dissolutiondissolved in THF (200 mL)
7. additionMethanol was added
8. distillationthe mixture was distilled at a constant volume of 350 mL, until THF
9. customhad been azeotropically removed
10. additionAdditional methanol (100 mL) was added
11. temperaturethe suspension was cooled to room temperature
12. filtrationThe solids were filtered
13. customdried under vacuum