Acetic Acid → N-benzyl-2-(pyrimidin-2-yl)ethanamine
反応式
[CH:1]([C:3]1[N:8]=[CH:7][CH:6]=[CH:5][N:4]=1)=[CH2:2].CC(O)=O.[CH2:13]([NH2:20])[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1>CCO>[CH2:13]([NH:20][CH2:2][CH2:1][C:3]1[N:8]=[CH:7][CH:6]=[CH:5][N:4]=1)[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1参加物
5
実験手順
To a solution of 2-vinylpyrimidine (1.55 g, 14.6 mmol) in EtOH (15 mL) at room temperature was added AcOH (2.0 mL) and benzylamine (3.14 g, 29.3 mmol) (3.2 mL). The reaction mixture was heated to reflux for 18 h, and concentrated. Diluted with EtOAc, washed with 5 M NaOH (1×), brine (1×), dried over MgSO4, filtered, and concentrated. Purification by flash column chromatography on silica gel (eluted with 2% to 10% MeOH in DCM) gave N-benzyl-2-(pyrimidin-2-yl)ethanamine.
後処理
- temperatureThe reaction mixture was heated
- temperatureto reflux for 18 h
- concentrationconcentrated
- additionDiluted with EtOAc
- washwashed with 5 M NaOH (1×), brine (1×)
- dry with materialdried over MgSO4
- filtrationfiltered
- concentrationconcentrated
- customPurification by flash column chromatography on silica gel (eluted with 2% to 10% MeOH in DCM)
出典と根拠
- ORDレコード
- ord-0d326be835d64035bb0f0b90796b21bf
- 出典データセット
- uspto-grants-2012_12
- 特許番号
- US08324396B2
反応ノート
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