Sodium Iodide → 5-Chloro-1-(3-iodopropyl)indole-3-carboxaldehyde
反応式
[Cl:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][CH:10]=1)[N:7]([CH2:11][CH2:12][CH2:13]Cl)[CH:6]=[C:5]2[CH:15]=[O:16].[I-:17].[Na+]>C(#N)C>[Cl:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][CH:10]=1)[N:7]([CH2:11][CH2:12][CH2:13][I:17])[CH:6]=[C:5]2[CH:15]=[O:16]参加物
4
実験手順
A stirred solution of 5-chloro-1-(3-chloropropyl)indole-3-carboxaldehyde (3.8 g, 15 mmol) and sodium iodide (4.5 g, 30 mmol) in acetonitrile (50 mL) under argon was heated under reflux for 18 h, cooled to room temperature and partitioned between ether (3×30 mL) and water (50 mL). The combined organic extracts were washed (aqueous sodium metabisulfite solution, water, brine), dried (sodium sulfate) and concentrated in vacuo to give the product as a yellow oil (5.0 g, 96%) which was used immediately.
後処理
- temperatureunder reflux for 18 h
- custompartitioned between ether (3×30 mL) and water (50 mL)
- washThe combined organic extracts were washed (aqueous sodium metabisulfite solution, water, brine)
- dry with materialdried (sodium sulfate)
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-0e7782ec23d24cd682978a095c17b783
- 出典データセット
- uspto-grants-2002_08
- 特許番号
- US06433175B1
反応ノート
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