Dimethylamine → 1-(6-Chloropyridin-3-yl)-N,N-dimethylmethanamine
反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8]Cl)=[CH:4][N:3]=1.[CH3:10][NH:11][CH3:12].C(=O)([O-])[O-].[K+].[K+].O>C(O)C>[Cl:1][C:2]1[N:3]=[CH:4][C:5]([CH2:8][N:11]([CH3:12])[CH3:10])=[CH:6][CH:7]=1参加物
6
実験手順
2-Chloro-5-(chloromethyl)pyridine (500 mg) was dissolved in ethanol (7.0 ml). dimethylamine (0.83 ml, 33% in ethanol) and potassium carbonate (641 mg) were added and the resulting mixture was refluxed for 1.5 hours. After evaboration of ethanol, water was added and the aqueous mixture was extracted with ethyl acetate. 1H NMR (400 MHz, d6-DMSO) δ: 8.31 (d, 1H, J 2.3 Hz), 7.77 (dd, 1H, J 8.2, 2.3 Hz), 7.47 (d, 1H, J 8.2 Hz), 3.41 (s, 2H), 2.14 (s, 6H).
後処理
- temperaturethe resulting mixture was refluxed for 1.5 hours
- extractionthe aqueous mixture was extracted with ethyl acetate
出典と根拠
- ORDレコード
- ord-a72f5db53d9240e08e12fcd5aba29a27
- 出典データセット
- uspto-grants-2009_01
- 特許番号
- US07482340B2
反応ノート
読み込み中…