反应详情

温度

80 °C

To a solution of 3-isopropyl-[1,2,4]triazolo[4,3-b]pyridazine-6-carbaldehyde (0.150 g, 0.789 mmol, Preparation #2) in 1,4-dioxane (3 mL) was added 1,4-difluoro-2-(isocyano(tosyl)methyl)benzene (0.202 g, 0.657 mmol, Preparation #4), K2CO3 (0.218 g, 1.58 mmol) and MeOH (3.00 mL). The reaction mixture was heated to about 80° C. for about 3 h. The reaction mixture was diluted with water (50 mL) and extracted with DCM (50 mL). The organic layer was dried with MgSO4, filtered and concentrated in vacuo. The crude material was purified by silica gel chromatography using heptane/EtOAc (gradient; 1:1 to 0:1) to give the title compound (0.161 g, 71% yield). LC/MS (Table 1, Method a) Rt=2.20 min; MS m/z: 342.1 (M+H)+.

1. extractionextracted with DCM (50 mL)
2. dry with materialThe organic layer was dried with MgSO4
3. filtrationfiltered
4. concentrationconcentrated in vacuo
5. customThe crude material was purified by silica gel chromatography