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

HRID 490203

反応式

HRID 490203 の反応式
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

参加物

4

反応物 2

HCID 4837PiperazineHCID 2208322-Bromo-3-methylpyridine

生成物 1

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

試薬・触媒・溶媒 1

HCID 2631-Butanol溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-574248bc234740a2bbf0875f2d8c86bc
出典データセット
uspto-grants-2009_05
特許番号
US07528134B2

関連ノート

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