Phosphorus oxychloride → 2-Chloroimidazo[1,2-a]pyridine-3-sulfonyl chloride
反応式
[Cl:1][C:2]1[N:3]=[C:4]2[CH:9]=[CH:8][CH:7]=[CH:6][N:5]2[C:10]=1[S:11]([OH:14])(=O)=[O:12].P(Cl)(Cl)([Cl:17])=O>>[Cl:1][C:2]1[N:3]=[C:4]2[CH:9]=[CH:8][CH:7]=[CH:6][N:5]2[C:10]=1[S:11]([Cl:17])(=[O:14])=[O:12]参加物
3
実験手順
2-Chloroimidazo[1,2-a]pyridine-3-sulfonic acid (5.0 g) is suspended in 30 ml of phosphorus oxychloride and refluxed for 5 hours. After cooling, the reaction solution is poured into 250 ml of ice water and extracted with dichloromethane. The dichloromethane layer is collected, dried on anydrous sodium sulfate and then concentrated to dryness under reduced pressure to afford 4.6 g of the title compound as pale yellowish crystals.
後処理
- temperaturerefluxed for 5 hours
- temperatureAfter cooling
- extractionextracted with dichloromethane
- customThe dichloromethane layer is collected
- dry with materialdried on anydrous sodium sulfate
- concentrationconcentrated to dryness under reduced pressure
出典と根拠
- ORDレコード
- ord-b91dec64a93c49ad9f6f4b6bc3ccd85c
- 出典データセット
- uspto-grants-1991_05
- 特許番号
- US05017212
反応ノート
読み込み中…