反应详情

温度

120 °C

2,3-Dichloro-5-nitropyridine (Synthesis, 1990, 6, 499-501) (20 g, 104 mmol) was added portionwise to morpholine (40 mL) at 0° C. and heated at 120° C. for 1 h. The reaction was cooled to room temperature, water (100 mL) added and the reaction extracted with DCM (3×150 mL). The organics were dried (MgSO4), filtered, and the solvent removed under reduced pressure to give the product as a yellow solid, which was triturated with isohexane and allowed to dry under vacuum at 60° C. 1H NMR δ 8.98 (1H, d), 8.47 (1H, d), 3.74-3.69 (4H, m), 3.67-3.62 (4H, m); MS m/e MH+ 244.

1. temperatureThe reaction was cooled to room temperature
2. extractionthe reaction extracted with DCM (3×150 mL)
3. dry with materialThe organics were dried (MgSO4)
4. filtrationfiltered
5. customthe solvent removed under reduced pressure