反应详情

温度

25 °C

To a flask containing a 4-bromopicolinic acid (1.0 g) in DMF (10 mL) was added HATU (2.3 g) and N-ethyl-N-isopropylpropan-2-amine (1.0 mL) The mixture was stirred at about 25° C. for approximately 10 min followed by addition of (4-methoxyphenyl)methanamine (0.68 g). The reaction was then stirred at about 25° C. for about an additional 12 h. The reaction was basified to pH 10 with aqueous 1 N NaOH and washed three times with EtOAc. The organic solution was dried over MgSO4, filtered, and concentrated under reduced pressure to afford 4-bromo-N-(4-methoxybenzyl)picolinamide as a clear oil (1.2 g, 75%). LC/MS (Table 1, method f). Rt=1.73 min; MS m/z 322 (M+H)+.

1. stirringThe reaction was then stirred at about 25° C. for about an additional 12 h
2. washwashed three times with EtOAc
3. dry with materialThe organic solution was dried over MgSO4
4. filtrationfiltered
5. concentrationconcentrated under reduced pressure