반응식
[Br:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH3:8])[C:3]=1[CH3:9].[Br:10]N1C(=O)CCC1=O.C(OOC(=O)C1C=CC=CC=1)(=O)C1C=CC=CC=1>ClC(Cl)(Cl)Cl>[Br:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH3:8])[C:3]=1[CH2:9][Br:10]참가 물질
5
실험 절차
A mixture of 3-bromo-o-xylene (15 g, 81 mmol), N-bromo succinimid (15.1 g, 85.1 mmol), dibenzoylperoxid (0.65 g) and tetrachloromethane (150 ml) was refluxed for 5 hours. After filtration the filtrate was washed with sodium hydrogensulfite and water. The organic layer was dried over sodium sulfate and evaporated in vacuo. Chromatography (SiO2) (petroleum ether:ethyl acetate, 100:4) gave a 16.8 g fraction of a mixture containing 45% of the title compound. This mixture was used without further purification.
후처리
- temperaturewas refluxed for 5 hours
- filtrationAfter filtration the filtrate
- washwas washed with sodium hydrogensulfite and water
- dry with materialThe organic layer was dried over sodium sulfate
- customevaporated in vacuo
- customChromatography (SiO2) (petroleum ether:ethyl acetate, 100:4) gave a 16.8 g fraction of a mixture
출처 및 근거
- ORD 기록
- ord-51db4384e25a49baa3d78657a3dfbb95
- 출처 데이터셋
- uspto-grants-2001_11
- 특허 번호
- US06313137B1
연결된 노트
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