Ethylamine → 2-(Ethylamino)-6fluoro-3-nitropyridine
반응식
F[C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][CH:5]=[C:4]([F:11])[N:3]=1.[CH2:12]([NH2:14])[CH3:13]>C1COCC1>[CH2:12]([NH:14][C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][CH:5]=[C:4]([F:11])[N:3]=1)[CH3:13]참가 물질
4
실험 절차
To a solution of 2,6-difluoro-3-nitropyridine (45.7 g, 285 mmol) in THF (500 mL) at −40° C. was added drop-wise a solution of ethylamine (25.7 g, 570 mmol) in THF (250 mL). After 30 min, the reaction mixture was concentrated under reduced pressure and the residue was dissolved in EtOAc. The organic phase was washed with brine, dried (MgSO4), filtered and concentrated. The resulting yellow solid was purified by flash chromatography (15% EtOAc in hexane) to give the title compound (43.2 g, 82% yield) as a yellow solid.
후처리
- concentrationthe reaction mixture was concentrated under reduced pressure
- dissolutionthe residue was dissolved in EtOAc
- washThe organic phase was washed with brine
- dry with materialdried (MgSO4)
- filtrationfiltered
- concentrationconcentrated
- customThe resulting yellow solid was purified by flash chromatography (15% EtOAc in hexane)
출처 및 근거
- ORD 기록
- ord-e4cf6ec97e3a42d592211acb955df550
- 출처 데이터셋
- uspto-grants-2002_07
- 특허 번호
- US06420359B1
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