反应详情

温度

0 °C

To a solution of 5-cyano-2-(difluoromethyl)nicotinic acid (0.600 g, 3.0 mmol) in dry DMF (20 mL), TBTU (10.0 g, 3.33 mmol) was added at 0° C. followed by slow addition of DIPEA (0.7 mL, 3.93 mmol). The reaction mass was stirred at 0° C. for 1 h and ammonium chloride (3.33 g, 60.7 mmol) was added. The reaction mass was stirred at RT for 30-48 h. After completion of reaction quenched the reaction mass with DCM, filtered off solid to afford 0.500 g of the desired product. 1H NMR (300 MHz, DMSO d6): δ 8.16 (m, 1H), 8.63 (s, 1H), 9.22 (s, 1H).

1. stirringThe reaction mass was stirred at RT for 30-48 h
2. customAfter completion of reaction
3. customquenched the reaction mass with DCM
4. filtrationfiltered off solid