Phosphorus oxychloride → 1,7-Dichloro-6-fluoroisoquinoline
반응식
[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]=1참가 물질
3
실험 절차
2.6 g (12.0 mmol) of 7-chloro-6-fluoro-isoquinoline 2-oxide (5) were heated in 40 ml of POCl3 at reflux for 4 h. After the mixture had 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 magnesium sulfate 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+).
후처리
- 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 magnesium sulfate
- customevaporated
출처 및 근거
- ORD 기록
- ord-7cf16209865744ce916f65461ff93d07
- 출처 데이터셋
- uspto-grants-2014_06
- 특허 번호
- US08742116B2
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