反应详情

3-Amino-1-propanol (4.5 g, 60.0 mmol) was added slowly to a mixture of 4-chloro-3-nitropyridine (8.0 g, 50.5 mmol) and sodium hydrogen carbonate (4.2 g, 50.0 mmol) in ethanol (200 ml). The mixture was stirred for 3 h at ambient temperature and the solvent removed under reduced pressure. Saturated aqueous sodium hydrogen carbonate (50 ml) was added to the residue, which was extracted with ethyl acetate (3×200 ml). The combined organics were dried over anhydrous sodium sulphate, filtered and evaporated. Crystallisation from ethyl acetate gave 4-(3-hydroxypropylamino)-3-nitropyridine (4.3 g, 43%) as an orange crystalline solid.

1. customthe solvent removed under reduced pressure
2. additionSaturated aqueous sodium hydrogen carbonate (50 ml) was added to the residue, which
3. extractionwas extracted with ethyl acetate (3×200 ml)
4. dry with materialThe combined organics were dried over anhydrous sodium sulphate
5. filtrationfiltered
6. customevaporated
7. customCrystallisation from ethyl acetate