反应详情

To a solution of 6-bromopyridin-2-amine (10 g, 57.79 mmol, 1 eq.) in 150 ml of DCM were added TEA (17.54 g, 173.3 mmol, 3 eq.) and 2,2-dimethylpropionyl chloride (10.45 g, 86.69 mmol, 1.5 eq.) dropwise. The temperature rose slowly. The reaction was stirred overnight at r.t. The white solid was removed by filtration and the solvent was evaporated. The crude was dissolved in with EtOAc and washed with 0.1N aq. HCl, sat. aqueous NaHCO3. The organics were dried over MgSO4 and concentrated. The resulting solid was recrystallized in EtOAc to give N-(6-bromopyridin-2-yl)-2,2-dimethylpropanamide (13.52 g, 91% yield) as a white solid.

1. customThe white solid was removed by filtration
2. customthe solvent was evaporated
3. dissolutionThe crude was dissolved in with EtOAc
4. washwashed with 0.1N aq. HCl, sat. aqueous NaHCO3
5. dry with materialThe organics were dried over MgSO4
6. concentrationconcentrated
7. customThe resulting solid was recrystallized in EtOAc