反应详情

温度

45 °C

Sodium hydride (60% in oil) (28 mg) was added to a DMF (2.4 ml) solution containing 5-bromo-N-methylnicotinamide (100 mg), followed by stirring at 45° C. for 1 hour. Methyl iodide (43 μl) was added under ice cooling, followed by stirring at room temperature for 1 hour. A saturated aqueous ammonium chloride solution and ethyl acetate were added to the reaction mixture. The organic layer was collected, washed with saturated saline, and dried over anhydrous magnesium sulfate. The solvent was distilled away under reduced pressure. Hexane was added to the obtained residue, solid matter was collected by filtration, and a white solid of 5-bromo-N,N-dimethylnicotinamide (42 mg) was thus obtained.

1. stirringby stirring at room temperature for 1 hour
2. customThe organic layer was collected
3. washwashed with saturated saline
4. dry with materialdried over anhydrous magnesium sulfate
5. distillationThe solvent was distilled away under reduced pressure
6. additionHexane was added to the obtained residue, solid matter
7. filtrationwas collected by filtration