Phosphorus oxychloride → 1,7-Dichloro-6-fluoroisoquinoline
反応式
[Cl:1][C:2]1[CH:11]=[C:10]2[C:5]([CH:6]=[CH:7][N+:8]([O-])=[CH:9]2)=[CH:4][C:3]=1[F:13].O=P(Cl)(Cl)[Cl:16]>>[Cl:16][C:9]1[C:10]2[C:5](=[CH:4][C:3]([F:13])=[C:2]([Cl:1])[CH:11]=2)[CH:6]=[CH:7][N:8]=1参加物
3
実験手順
2.6 g (12.0 mmol) of 7-Chloro-6-fluoro-isoquinoline 2-oxide (4) were heated in 40 ml of POCl3 at reflux for 4 h. After the mixture has cooled down to room temperature, it was poured on ice. The aqueous solution was extracted three times with dichloromethane. The combined organic layers were dried with MgSO4 and evaporated to yield 2.91 g of the title compound, which was used without further purification. Rt=2.34 min (Method A). Detected mass: 216.0/218.0 (M+H+).
後処理
- temperatureat reflux for 4 h
- additionit was poured on ice
- extractionThe aqueous solution was extracted three times with dichloromethane
- dry with materialThe combined organic layers were dried with MgSO4
- customevaporated
出典と根拠
- ORDレコード
- ord-9cc687742f6840248303f47a2f99ad90
- 出典データセット
- uspto-grants-2013_06
- 特許番号
- US08461144B2
反応ノート
読み込み中…