Piperazine → 1-(3-Methyl-2-pyridinyl)piperazine

HRID 490203

반응식

HRID 490203 반응식
Br[C:2]1[C:7]([CH3:8])=[CH:6][CH:5]=[CH:4][N:3]=1.[NH:9]1[CH2:14][CH2:13][NH:12][CH2:11][CH2:10]1>C(O)CCC>[CH3:8][C:7]1[C:2]([N:9]2[CH2:14][CH2:13][NH:12][CH2:11][CH2:10]2)=[N:3][CH:4]=[CH:5][CH:6]=1

참가 물질

4

반응물 2

HCID 4837PiperazineHCID 2208322-Bromo-3-methylpyridine

생성물 1

HCID 27600571-(3-Methyl-2-pyridinyl)piperazine

시약·촉매·용매 1

HCID 2631-Butanol용매

실험 절차

To a slurry of 2-bromo-3-methylpyridine (3.30 mL, 29.6 mmol) in n-butanol was added piperazine (25.0 g, 290 mmol) and the reaction heated to reflux for 3 days. The mixture was cooled and the solvent removed under reduced pressure. The residue was partitioned between water and ethyl acetate. The organic phase was dried (sodium sulfate) and concentrated. The residue was purified by flash column chromatography on silica gel (elution with 15% methanol:dichloromethane) to provide the title compound as a yellow oil.

후처리

  1. temperaturethe reaction heated
  2. temperatureto reflux for 3 days
  3. temperatureThe mixture was cooled
  4. customthe solvent removed under reduced pressure
  5. customThe residue was partitioned between water and ethyl acetate
  6. dry with materialThe organic phase was dried (sodium sulfate)
  7. concentrationconcentrated
  8. customThe residue was purified by flash column chromatography on silica gel (elution with 15% methanol:dichloromethane)

출처 및 근거

ORD 기록
ord-574248bc234740a2bbf0875f2d8c86bc
출처 데이터셋
uspto-grants-2009_05
특허 번호
US07528134B2

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