Pyridine → 1-o-Tolyl-propane-1,2-dione
반응식
[C:1]1([CH3:11])[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[CH2:7][C:8](=[O:10])[CH3:9].[Cr](Cl)([O-])(=O)=[O:13].[NH+]1C=CC=CC=1.N1C=CC=CC=1>C(Cl)Cl>[C:1]1([CH3:11])[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[C:7](=[O:13])[C:8](=[O:10])[CH3:9]참가 물질
5
실험 절차
A mixture of 7 g (47.23 mmol) 1-o-Tolyl-propan-2-one, 30.5 g (0.141 mol) pyridinium chlorochromate and 11.2 g (0.141 mol) pyridine in 200 ml DCM was heated to reflux for 16 h. The mixture was filtered through a pad of silica and the filtrate was evaporated under reduced pressure. The residue was purified by flash column chromatography on silica eluting with ethyl acetate/n-hexane 1:4. The product fractions were evaporated to yield 1.178 g (15%) of the title compound.
후처리
- temperaturewas heated
- temperatureto reflux for 16 h
- filtrationThe mixture was filtered through a pad of silica
- customthe filtrate was evaporated under reduced pressure
- customThe residue was purified by flash column chromatography on silica eluting with ethyl acetate/n-hexane 1:4
- customThe product fractions were evaporated
출처 및 근거
- ORD 기록
- ord-d3283aa22633440c9c72b26f773945fc
- 출처 데이터셋
- uspto-grants-2004_02
- 특허 번호
- US06686381B2
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