Piperidine → 1-(5-Fluoro-2-nitrophenyl)piperidine
反応式
F[C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[N+:9]([O-:11])=[O:10].[NH:12]1[CH2:17][CH2:16][CH2:15][CH2:14][CH2:13]1>CCO>[F:8][C:6]1[CH:5]=[CH:4][C:3]([N+:9]([O-:11])=[O:10])=[C:2]([N:12]2[CH2:17][CH2:16][CH2:15][CH2:14][CH2:13]2)[CH:7]=1参加物
4
実験手順
To a solution of 2,4-difluoronitrobenzene (2.09 g, 13.1 mmol) in EtOH (10 mL) at ambient temperature was added piperidine (3.35 g, 39.4 mmol) dropwise. The reaction was allowed to stir overnight and concentrated in vacuo. The residue was dissolved in EtOAc (100 mL), washed with water (2×100 mL), dried (Na2SO4) and concentrated in vacuo. Purification by silica gel column chromatography afforded 1.10 (37%) of the title compound as an oil. Mass spectrum (ESI, m/z): Calcd. for C11H13FN2O2, 225.1 (M+H), found 225.1.
後処理
- concentrationconcentrated in vacuo
- dissolutionThe residue was dissolved in EtOAc (100 mL)
- washwashed with water (2×100 mL)
- dry with materialdried (Na2SO4)
- concentrationconcentrated in vacuo
- customPurification by silica gel column chromatography
出典と根拠
- ORDレコード
- ord-73ecc3b717224c47a915a4cc25aca307
- 出典データセット
- uspto-grants-2008_09
- 特許番号
- US07427683B2
反応ノート
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