Phosphorus oxychloride → 4-Chloro-6-iodoquinoline-3-carbonitrile
反応式
[I:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[NH:8][CH:7]=[C:6]([C:12]#[N:13])[C:5]2=O.P(Cl)(Cl)([Cl:17])=O>>[Cl:17][C:5]1[C:4]2[C:9](=[CH:10][CH:11]=[C:2]([I:1])[CH:3]=2)[N:8]=[CH:7][C:6]=1[C:12]#[N:13]参加物
3
実験手順
A mixture of 6 6-iodo-4-oxo-1,4-dihydro-quinoline-3-carbonitrile (example 14b) (100 g, 0.34 mol) in phosphorus oxychloride (300 mL) was refluxed under N2 for 7 h. After cooling, the solvent was removed by rotary evaporator and then by the oil pump. Sat. sodium bicarbonate (200 mL) and ice water were slowly added. The solid was collected by filtration, washed with sat. sodium bicarbonate, water and dried to obtain 4-chloro-6-iodo-quinoline-3-carbonitrile (58 g, 98%) as a yellow solid. LC-MS m/e 315 (MH+).
後処理
- temperaturewas refluxed under N2 for 7 h
- temperatureAfter cooling
- customthe solvent was removed by rotary evaporator
- additionSat. sodium bicarbonate (200 mL) and ice water were slowly added
- filtrationThe solid was collected by filtration
- washwashed with sat. sodium bicarbonate, water
- customdried
出典と根拠
- ORDレコード
- ord-2fda928f72ed4c278ade8f07219a366f
- 出典データセット
- uspto-grants-2007_07
- 特許番号
- US07250515B2
反応ノート
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