반응 #9730

반응 방정식

Bromine

methyl 2-methyl-3-furancarboxylate

sodium thiosulfate

→

title compound

methyl 5-bromo-2-methyl-3-furoate

용매

1,4-dioxane

반응 조건

후처리

1. 1
   workup.STIRRINGStirring
2. 2
   workup.WAITat ambient temperature for 18 hours
3. 3
   추출was then extracted with ethyl acetate
4. 4
   건조The organic layer was dried with brine and over magnesium sulfate
5. 5
   기타The product isolated
6. 6
   기타after evaporation of the solvent
7. 7
   기타was further purified by flash column chromatography

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.

출처