反応 #50772

反応方程式

3-Amino-1-propanol

4-chloro-3-nitropyridine

sodium hydrogen carbonate

→

4-(3-hydroxypropylamino)-3-nitropyridine

収率 43.2%

溶媒

ethanol

反応条件

後処理

1. 1
   その他the solvent removed under reduced pressure
2. 2
   workup.ADDITIONSaturated aqueous sodium hydrogen carbonate (50 ml) was added to the residue, which
3. 3
   抽出was extracted with ethyl acetate (3×200 ml)
4. 4
   乾燥The combined organics were dried over anhydrous sodium sulphate
5. 5
   ろ過filtered
6. 6
   その他evaporated
7. 7
   その他Crystallisation from ethyl acetate

実験手順

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.

出典