反应详情

温度

100 °C

To a solution of 3-benzyl-6-chloro-4,5-dimethylpyridazine (800 mg, 3.44 mmol) in 20 mL DMF is added tert-butyl 4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-5,6-dihydropyridine-1(2H)-carboxylate (1.3 g, 4.1 mmol), followed with potassium carbonate (1.43 g, 10.3 mmol) and Pd(PPh3)4 (397 mg, 0.344 mmol) in a round bottom flask. The vial is evacuated and flushed with nitrogen. The reaction mixture is heated to 100° C. for 16 h. The mixture is filtered through Celite and the filtrate is concentrated to afford the crude material. The mixture is purified by flash chromatography on silica gel, eluting with 3%-15% MeOH: DCM. Fractions containing the desired product are combined and concentrated to afford a brown solid (1.0 g, 77%).

1. customThe vial is evacuated
2. customflushed with nitrogen
3. filtrationThe mixture is filtered through Celite
4. concentrationthe filtrate is concentrated
5. customto afford the crude material
6. customThe mixture is purified by flash chromatography on silica gel
7. washeluting with 3%-15% MeOH
8. additionFractions containing the desired product
9. concentrationconcentrated