Hydrochloric Acid → 1-(4-isopropoxyphenyl)propan-2-one
반응식
Cl.[CH:2]([O:5][C:6]1[CH:11]=[CH:10][C:9]([CH:12]=[C:13]([N+]([O-])=O)[CH3:14])=[CH:8][CH:7]=1)([CH3:4])[CH3:3].[O:18]1CCCC1>[Fe]>[CH:2]([O:5][C:6]1[CH:11]=[CH:10][C:9]([CH2:12][C:13](=[O:18])[CH3:14])=[CH:8][CH:7]=1)([CH3:4])[CH3:3]참가 물질
5
실험 절차
Concentrated hydrochloric acid (90 ml) was added dropwise, over 45 minutes, to a stirred mixture of iron powder (17.5 g) and 1-(4-isopropoxyphenyl)-2-nitroprop1-ene (16.0 g) in tetrahydrofuran (50 ml) at reflux. The mixture was heated under reflux for a further hour, cooled, filtered through diatomaecous earth and the tetrahydrofuran removed under reduced pressure. The residue was diluted with water, extracted with diethyl ether, washed with brine, dried (magnesium sulphate), filtered and evaporated to dryness. Distillation of the residue gave the title compound, bp 120°-6°/1.5 mm.
후처리
- temperatureat reflux
- temperatureThe mixture was heated
- temperatureunder reflux for a further hour
- temperaturecooled
- filtrationfiltered through diatomaecous earth
- customthe tetrahydrofuran removed under reduced pressure
- additionThe residue was diluted with water
- extractionextracted with diethyl ether
- washwashed with brine
- dry with materialdried (magnesium sulphate)
- filtrationfiltered
- customevaporated to dryness
- distillationDistillation of the residue
출처 및 근거
- ORD 기록
- ord-c20dbfec2e004b3f8259191b0db34ffc
- 출처 데이터셋
- uspto-grants-1986_11
- 특허 번호
- US04622342
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