反应详情

To a solution of 5′-methyl-5-(1-pyrrolidinyl)-2,3′-bipyridine-4-carboxylic acid (2-2, 0.026 g, 0.085 mmol) and 1-(5,6-dimethoxy-2-pyridinyl)methanamine (3-6, 0.017 g, 0.102 mmol) in DMF (0.17 mL) was added HATU (0.032 g, 0.085 mmol) followed by DEA (0.074 mL, 0.426 mmol) and stirred at ambient temperature for 1 h. The system was partitioned between saturated aqueous sodium bicarbonate and EtOAc, washed with brine and dried over magnesium sulfate. Filtration and concentration followed by purification via normal phase chromatography (0→10% MeOH in EtOAc) afforded the title compound (2-3) as a salmon powder. 1H NMR (500 MHz, CDCl3) δ 8.93 (s, 1H), 8.40 (m, 1H), 8.32 (s, 1H), 8.06 (m, 1H), 7.08 (s, 1H), 7.06 (d, 1H, J=8.0 Hz), 6.90 (d, 1H, J=8.0 Hz), 4.63 (d, 2H, J=4.5 Hz), 4.00 (s, 3H), 3.89 (s, 3H), 3.36 (m, 4H), 2.40 (s, 3H), 1.93 (m, 4H). HRMS[M+H]C24H22N5O3 calc'd 434.2187. found 434.2211.

1. customThe system was partitioned between saturated aqueous sodium bicarbonate and EtOAc
2. washwashed with brine
3. dry with materialdried over magnesium sulfate
4. filtrationFiltration and concentration
5. customfollowed by purification via normal phase chromatography (0→10% MeOH in EtOAc)