反应详情

A mixture of pyridazin-3-ylamine (2 g, 21.05 mmol) and (3-bromo-1-methyl-2-oxopropyl)-carbamic acid benzyl ester (7.5 g, 25.26 mmol) in EtOH (25 mL) was heated to reflux overnight. After completion, the reaction mixture was cooled to rt. EtOH was removed in vacuo. The residue was dissolved in EtOAc. The organic layer was dried over sodium sulfate, filtered and concentrated in vacuo. The crude product was purified by column chromatography using silica gel (100-200 mesh) and 0-5% MeOH in DCM to provide (1-imidazo[1,2-b]pyridazin-2-yl-ethyl)-carbamic acid benzyl ester: LC-MS (ESI) m/z 297.3 [M+H]+.

1. temperaturewas heated
2. temperatureto reflux overnight
3. customEtOH was removed in vacuo
4. dissolutionThe residue was dissolved in EtOAc
5. dry with materialThe organic layer was dried over sodium sulfate
6. filtrationfiltered
7. concentrationconcentrated in vacuo
8. customThe crude product was purified by column chromatography