Piperidine → 1-(5-Fluoro-2-nitrophenyl)piperidine

HRID 32893

反応式

HRID 32893 の反応式
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

反応物 2

HCID 8082PiperidineHCID 679672,4-Difluoronitrobenzene

生成物 1

HCID 532567081-(5-Fluoro-2-nitrophenyl)piperidine

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

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

  1. concentrationconcentrated in vacuo
  2. dissolutionThe residue was dissolved in EtOAc (100 mL)
  3. washwashed with water (2×100 mL)
  4. dry with materialdried (Na2SO4)
  5. concentrationconcentrated in vacuo
  6. 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

関連ノート

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