Bromine → Methyl 5-bromo-2-methylfuran-3-carboxylate
反応式
[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]=1参加物
5
反応条件
- 温度
- 0 °C
実験手順
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.
後処理
- 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
出典と根拠
- ORDレコード
- ord-f33b834f86d64fcebdaf4b4e0d91a9c5
- 出典データセット
- uspto-grants-2006_08
- 特許番号
- US07091237B2
反応ノート
読み込み中…