反应详情

温度

80 °C

Sodium hydride (60%, 120 mg, 3 mmol) was added to a solution of Intermediate P (1.21 g, 2.0 mmol) and 5-fluoro-2-pyridinecarbonitrile (0.61 g, 5.0 mmol) in anhydrous dimethylformamide (20 mL), stirred under argon, and the obtained mixture was heated at 80° C. for 16 hours. The reaction mixture was poured into ice/water (200 mL), and extracted with dichloromethane (200 mL). The extract was dried over sodium sulfate, and the solvent was evaporated. The residue was diluted with chlorobenzene (50 mL), and the volatiles were removed under high vacuum. The crude product was purified by chromatography (dichloromethane/hexane 2:1) to give 4,7-bis(4-(N,N-diphenylamino)phenyl)-2-(6-cyanopyridin-3-yl)-2H-benzo[d][1,2,3]triazole, dark-red crystals, 1.20 g (85%).

1. extractionextracted with dichloromethane (200 mL)
2. dry with materialThe extract was dried over sodium sulfate
3. customthe solvent was evaporated
4. additionThe residue was diluted with chlorobenzene (50 mL)
5. customthe volatiles were removed under high vacuum
6. customThe crude product was purified by chromatography (dichloromethane/hexane 2:1)