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

HRID 32893

반응식

HRID 32893 반응식
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

참가 물질

4

반응물 2

HCID 8082PiperidineHCID 679672,4-Difluoronitrobenzene

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-73ecc3b717224c47a915a4cc25aca307
출처 데이터셋
uspto-grants-2008_09
특허 번호
US07427683B2

연결된 노트

불러오는 중…