Chloroacetaldehyde → 7-Ethylimidazo[1,2-a]pyridine
反応式
[CH2:1]([C:3]1[CH:8]=[CH:7][N:6]=[C:5]([NH2:9])[CH:4]=1)[CH3:2].Cl[CH2:11][CH:12]=O>CCO>[CH2:1]([C:3]1[CH:8]=[CH:7][N:6]2[CH:11]=[CH:12][N:9]=[C:5]2[CH:4]=1)[CH3:2]参加物
4
実験手順
A mixture of 4-ethylpyridin-2-amine (3.21 g, 8.19 mmol), and chloroacetaldehyde (50% aqueous solution, 2.6 ml, 10.5 mmol) in EtOH (10 ml) was refluxed vigorously for 12 hours. The reaction mixture was concentrated, and the residue was suspended in saturated aqueous sodium bicarbonate solution. The aqueous mixture was extracted with CH2Cl2 and EtOAc, and the combined organic extracts were dried over Na2SO4, filtered and concentrated to afford the desired product (1.18 g, 98% yield) as a viscous oil. MS APCI (+) m/z 147.2 (M+1) detected.
後処理
- temperaturewas refluxed vigorously for 12 hours
- concentrationThe reaction mixture was concentrated
- extractionThe aqueous mixture was extracted with CH2Cl2 and EtOAc
- dry with materialthe combined organic extracts were dried over Na2SO4
- filtrationfiltered
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-a14ef65495744592aceb2fbe75dcfb13
- 出典データセット
- uspto-grants-2012_03
- 特許番号
- US08138181B2
反応ノート
読み込み中…