反应详情

To a round bottom flask was added 1-(2,4-difluorophenyl)-2-(3-isopropyl-[1,2,4]triazolo[4,3-b]pyridazin-6-yl)ethanone (1.50 g, 4.74 mmol, Preparation #K.1) followed by DMSO (15 mL) and NBS (0.844 g, 4.74 mmol). The reaction mixture was stirred at about ambient temperature for about 3 d. The reaction mixture was partitioned between EtOAc and water. The layers were separated, and the organic layer was washed with brine, dried over MgSO4, filtered, and concentrated in vacuo. The crude material was purified by silica gel chromatography using heptane/EtOAc (gradient, 1:0 to 0:1) to give the title compound (1.14 g, 73%): LC/MS (Table 1, Method a) Rt=2.4 min; MS m/z: 331.1 (M+H)+.

1. customThe reaction mixture was partitioned between EtOAc and water
2. customThe layers were separated
3. washthe organic layer was washed with brine
4. dry with materialdried over MgSO4
5. filtrationfiltered
6. concentrationconcentrated in vacuo
7. customThe crude material was purified by silica gel chromatography