反应详情

To a solution of Imidazo[1,2-a]pyridine-7-carboxylic acid methyl ester (0.67 g, 3.83 mmol) and dimethylhydroxylamine (0.93 g, 9.57 mmol) in CH2Cl2 (40 ml) at 0° C. was added 2M trimethylaluminium solution in hexane (3.8 ml, 9.57 mmol). The reaction mixture was allowed to warm to room temperature and stirred for 1 h, before being cooled back to 0° C. and quenched with ice. The reaction was filtered and liquid fraction partitioned between CH2Cl2/H2O. The organic layer was separated, dried (MgSO4), filtered and the solvent removed in vacuo to afford the crude product. The residue was purified by silica column chromatography (0-50% MeOH in Et2O) to afford the product (187 mg). MS: [M+H]+=206.

1. temperaturebefore being cooled back to 0° C.
2. customquenched with ice
3. filtrationThe reaction was filtered
4. customliquid fraction partitioned between CH2Cl2/H2O
5. customThe organic layer was separated
6. dry with materialdried (MgSO4)
7. filtrationfiltered
8. customthe solvent removed in vacuo
9. customto afford the crude product
10. customThe residue was purified by silica column chromatography (0-50% MeOH in Et2O)