Dimethylamine → HCID 22282638、化合物
反応式
Br[C:2]1[CH:11]=[C:10]([Br:12])[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[N:3]=1.[CH3:13][NH:14][CH3:15]>CCO>[Br:12][C:10]1[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[N:3]=[C:2]([N:14]([CH3:15])[CH3:13])[CH:11]=1参加物
4
実験手順
A solution of 2,4-dibromoquinoline (273 mg, 1.0 mmol) in EtOH (15 mL) was treated with aqueous dimethylamine (40%, 0.4 mL, 3 mmol), stirred at room temperature for 16 h, concentrated in vacuo and purified by chromatography [SiO2; heptane-EtOAc (9:1)] to give the product (119 mg, 50%) as a cream solid: IR νmax (Nujol)/cm−1 2924, 2854, 1598, 1546, 1510, 1463, 1379 and 754; NMR δH (400 MHz, CDCl3) 3.21 (6H, s), 7.21 (1H, s), 7.23-7.26 (1H, m), 7.55 (1H, t, J 8.2 Hz), 7.68 (1H, d, J 8.5 Hz) and 7.94 (1H, d, J 7.1 Hz); M/Z 251 (M+H)+.
後処理
- concentrationconcentrated in vacuo
- custompurified by chromatography [SiO2; heptane-EtOAc (9:1)]
出典と根拠
- ORDレコード
- ord-d68cbca7fb61459bb6647eab92a2ebfe
- 出典データセット
- uspto-grants-2003_06
- 特許番号
- US06583156B1
反応ノート
読み込み中…