反应详情

温度

0 °C

A mixture of 8-bromo-6-chloroimidazo[1,2-b]pyridazine (214 mg, 921 μmol, Eq: 0.95) and 5-((4-methylpiperazin-1-yl)methyl)pyridin-2-amine (200 mg, 970 μmol, Eq: 1.00) in DMF (10.0 ml) was cooled to 0° C. To this was added sodium hydride (60% in mineral oil, 124 mg, 3.1 mmol, Eq: 3.2). The reaction was allowed to stir at 0° C. for 10 min and then allowed to warm to room temperature and stirred for 72 h. The reaction was quenched with saturated NaHCO3 (aq) and then diluted with water and EtOAc. The organic layer was separated and the aqueous phase was washed with EtOAc. The organic layers were combined, dried over MgSO4 and concentrated in vacuo. The residue was dissolved in Et2O. The organic layer was washed with water and dried over MgSO4. The drying agent was removed by filtration. The resulting solution was concentrated in vacuo to give (6-chloro-imidazo[1,2-b]pyridazin-8-yl)-[5-(4-methyl-piperazin-1-ylmethyl)-pyridin-2-yl]-amine (170 mg, 49%) as a solid. LC/MS-ESI observed [M+H]+ 358.

1. temperatureto warm to room temperature
2. stirringstirred for 72 h
3. customThe reaction was quenched with saturated NaHCO3 (aq)
4. additiondiluted with water and EtOAc
5. customThe organic layer was separated
6. washthe aqueous phase was washed with EtOAc
7. dry with materialdried over MgSO4
8. concentrationconcentrated in vacuo
9. dissolutionThe residue was dissolved in Et2O
10. washThe organic layer was washed with water
11. dry with materialdried over MgSO4
12. customThe drying agent was removed by filtration
13. concentrationThe resulting solution was concentrated in vacuo