反应详情

温度

100 °C

A mixture of 2-chloro-5-nitroisonicotinic acid (28.5 g, 141 mmol), morpholine (36.8 g, 423 mmol) and k2CO3 (58.4 g, 423 mmol) was stirred at 100° C. for 4 h. The mixture was cooled to room temperature and poured into water (1.5 L). It was acidified with 4N HCl to pH=1 and extracted with EA (1 L×3). The combined organic layers were washed with brine (1 L×5), then dried over anhydrous Na2SO4, filtered and concentrated in vacuo to afford the desired product as a yellow solid (27 g, 76%); LC/MS: MS (ES+) m/e 254 (MH+); 1H NMR (300 MHz, DMSO-d6) δ ppm 3.68 (t, J=4.8 Hz, 1H), 3.77 (t, J=4.8 Hz, 4H), 6.99 (s, 1H), 8.91 (s, 1H).

1. temperatureThe mixture was cooled to room temperature
2. extractionextracted with EA (1 L×3)
3. washThe combined organic layers were washed with brine (1 L×5)
4. dry with materialdried over anhydrous Na2SO4
5. filtrationfiltered
6. concentrationconcentrated in vacuo