Ethylamine → N-Ethyl-3-nitropyridin-4-amine
반응식
Cl.CO[C:4]1[CH:9]=[CH:8][N:7]=[CH:6][C:5]=1[N+:10]([O-:12])=[O:11].[CH2:13]([NH2:15])[CH3:14]>C(O)C.O>[CH2:13]([NH:15][C:4]1[CH:9]=[CH:8][N:7]=[CH:6][C:5]=1[N+:10]([O-:12])=[O:11])[CH3:14]참가 물질
5
실험 절차
4-Methoxy-3-nitropyridine hydrochloride (11.2 g, 58.9 mmol) in ethanol (75 ml) was treated with a 70% solution of ethylamine in water (64 ml) and heated under reflux for 2 hours. After cooling to room temperature, the solvent was removed in vacuo and the residue dissolved in ethyl acetate and water. The mixture was extracted (×3) with ethyl acetate, washed with water and saturated aqueous sodium chloride solution before drying over magnesium sulfate. Evaporation of the solvent afforded the title compound (11.7 g, 96%).
후처리
- temperatureheated
- temperatureunder reflux for 2 hours
- customthe solvent was removed in vacuo
- dissolutionthe residue dissolved in ethyl acetate
- extractionThe mixture was extracted (×3) with ethyl acetate
- washwashed with water and saturated aqueous sodium chloride solution
- dry with materialbefore drying over magnesium sulfate
- customEvaporation of the solvent
출처 및 근거
- ORD 기록
- ord-c98222fc8f0f467294076e546512ad1b
- 출처 데이터셋
- uspto-grants-2009_10
- 특허 번호
- US07598251B2
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