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[CH3:1][O:2][C:3]1[C:16]([O:17][CH3:18])=[CH:15][C:6]([CH2:7][O:8][CH2:9][CH2:10][CH2:11][CH2:12][CH:13]=[CH2:14])=[C:5]([N+:19]([O-:21])=[O:20])[CH:4]=1.[CH3:22][O:23][SiH:24]([O:27][CH3:28])[O:25][CH3:26]>[H+].[H+].O.O.O.O.O.O.Cl[Pt-2](Cl)(Cl)(Cl)(Cl)Cl>[CH3:22][O:23][Si:24]([O:27][CH3:28])([O:25][CH3:26])[CH2:14][CH2:13][CH2:12][CH2:11][CH2:10][CH2:9][O:8][CH2:7][C:6]1[CH:15]=[C:16]([O:17][CH3:18])[C:3]([O:2][CH3:1])=[CH:4][C:5]=1[N+:19]([O-:21])=[O:20]참가 물질
반응 조건
- 온도
- 37 °C
실험 절차
A 20-ml eggplant type flask was purged with nitrogen, and charged with 2.95 g (10.0 mmol) of 5-hexenyl 4,5-dimethoxy-2-nitrobenzyl ether, 1.47 g (12 mmol) of trimethoxysilane, and an infinitesimal amount of hydrogen hexachloroplatinate(IV) hexahydrate (H2PtCl6·6H2O), followed by stirring at 37° C. for 30 minutes. Thereafter, the bath temperature was raised to 100° C., and the reaction was completed in 2 hours. The reaction mixture was purified by silica gel column chromatography using a medium-pressure column. Using a mixture of hexane, ethyl acetate and tetramethoxysilane (in a volume ratio of 100:20:1) as the eluent, 1.4 g (3.35 mmol) of the desired product was obtained in a 34% yield. Its Rf value (for the aforesaid eluent) was 0.1.
후처리
- customA 20-ml eggplant type flask was purged with nitrogen
- temperatureThereafter, the bath temperature was raised to 100° C.
- waitthe reaction was completed in 2 hours
- customThe reaction mixture was purified by silica gel column chromatography
- additiona mixture of hexane, ethyl acetate and tetramethoxysilane (in a volume ratio of 100:20:1) as the eluent
출처 및 근거
- ORD 기록
- ord-e216d9f937914b04ab8c2a7b83608be9
- 출처 데이터셋
- uspto-grants-2006_09
- 특허 번호
- US07112397B2
연결된 노트
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