Bromine → Methyl 5-bromo-2-methylfuran-3-carboxylate
반응식
[Br:1]Br.[CH3:3][C:4]1[O:5][CH:6]=[CH:7][C:8]=1[C:9]([O:11][CH3:12])=[O:10].S([O-])([O-])(=O)=S.[Na+].[Na+]>O1CCOCC1>[Br:1][C:6]1[O:5][C:4]([CH3:3])=[C:8]([C:9]([O:11][CH3:12])=[O:10])[CH:7]=1참가 물질
5
반응 조건
- 온도
- 0 °C
실험 절차
Bromine (2.0 ml) was added drop-wise to a mixture of methyl 2-methyl-3-furancarboxylate (5.0 g) in 1,4-dioxane (35 ml) stirred at 0° C. Stirring was continued at 0° C. for 2 hours and then at ambient temperature for 18 hours. Saturated aqueous sodium thiosulfate was added to the reaction mixture which was then extracted with ethyl acetate. The organic layer was dried with brine and over magnesium sulfate. The product isolated after evaporation of the solvent was further purified by flash column chromatography using cyclohexane:ethyl acetate (19:1) as eluent to give the title compound as a yellow oil.
후처리
- stirringStirring
- waitat ambient temperature for 18 hours
- extractionwas then extracted with ethyl acetate
- dry with materialThe organic layer was dried with brine and over magnesium sulfate
- customThe product isolated
- customafter evaporation of the solvent
- customwas further purified by flash column chromatography
출처 및 근거
- ORD 기록
- ord-f33b834f86d64fcebdaf4b4e0d91a9c5
- 출처 데이터셋
- uspto-grants-2006_08
- 특허 번호
- US07091237B2
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