反応式
[NH2:1][C:2]1[CH:9]=[CH:8][C:5]([C:6]#N)=[CH:4][CH:3]=1.Cl.[CH3:11][NH:12][CH2:13][CH2:14][NH2:15]>CO>[CH3:11][N:12]1[CH2:13][CH2:14][N:15]=[C:6]1[C:5]1[CH:8]=[CH:9][C:2]([NH2:1])=[CH:3][CH:4]=1参加物
5
実験手順
To a solution of 4-aminobenzonitrile (5.1 g, 43 mmol) in dry methanol (60 mL) at 0 C, hydrogen chloride gas was bubbled through until saturation was reached. The mixture was then stirred at room temperature overnight. It was concentrated in vacuo. The residue was dissolved in dry methanol (60 mL). To the solution, N-methyl ethylenediamine (19 mL, 216 mmol) was added. The mixture was then heated to reflux for 3 h. After being cooled in fridge overnight, the precipitated product was collected by filtration, then was dried on vacuum to give white solids (3.7 g). MS 176.0 (M+H).
後処理
- concentrationIt was concentrated in vacuo
- dissolutionThe residue was dissolved in dry methanol (60 mL)
- temperatureThe mixture was then heated
- temperatureto reflux for 3 h
- temperatureAfter being cooled in fridge overnight
- filtrationthe precipitated product was collected by filtration
- customwas dried on vacuum
出典と根拠
- ORDレコード
- ord-6fd288883ee34f8499d1fd52141b360a
- 出典データセット
- uspto-grants-2010_03
- 特許番号
- US07678913B2
関連ノート
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