Ethylamine → 2-(Ethylamino)-6fluoro-3-nitropyridine
反応式
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]参加物
4
実験手順
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.
後処理
- 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)
出典と根拠
- ORDレコード
- ord-e4cf6ec97e3a42d592211acb955df550
- 出典データセット
- uspto-grants-2002_07
- 特許番号
- US06420359B1
反応ノート
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