Phosphorus oxychloride → HCID 10384366, 화합물
반응식
[C:1]([C:6]1[C:15](=O)[C:14]2[C:9](=[C:10]([CH2:17][O:18][C:19](=[O:26])[C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=3)[CH:11]=[CH:12][CH:13]=2)[NH:8][CH:7]=1)(=[O:5])[CH:2]([CH3:4])[CH3:3].P(Cl)(Cl)([Cl:29])=O>>[C:1]([C:6]1[CH:7]=[N:8][C:9]2[C:14]([C:15]=1[Cl:29])=[CH:13][CH:12]=[CH:11][C:10]=2[CH2:17][O:18][C:19](=[O:26])[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1)(=[O:5])[CH:2]([CH3:4])[CH3:3]참가 물질
3
실험 절차
A solution of 3-isobutyryl-8-(benzoyloxymethyl)-4(1H)-quinolone (11.81 g, 29.9 mmol) in phosphoryl chloride (100 ml) was heated at reflux for 2.5 hours, then the excess phosphoryl chloride evaporated. Water was added and the product extracted into a mixture of dichloromethane and isopropyl alcohol. Drying and evaporation of the organic layer gave crude 3-isobutyryl-4-chloro-8-(benzoyloxymethyl)quinoline (12.0 g), contaminated with isopropyl alcohol. This was used without further purification.
후처리
- temperatureat reflux for 2.5 hours
- customthe excess phosphoryl chloride evaporated
- additionWater was added
- extractionthe product extracted into a mixture of dichloromethane and isopropyl alcohol
- customDrying
- customevaporation of the organic layer
출처 및 근거
- ORD 기록
- ord-92aa79ba937f4fa896c79849779d1753
- 출처 데이터셋
- uspto-grants-1995_07
- 특허 번호
- US05432182
반응 노트
불러오는 중…