反应详情

3-Methyl-thiophene-2-carboxylic acid methyl ester (1 g, 6.4 mmol) is dissolved in CCl4 (15 mL), and NBS (1.19 g, 6.7 mmol) and benzoyl peroxide (15 mg) are added. The reaction mixture is refluxed for 6 hours, then water is added and the mixture is extracted with EtOAc (3×). The organic layers are dried over MgSO4, filtered and concentrated. The crude product is purified by silica gel column chromatography eluting with 98:2 petroleum ether-EtOAc to give the title compound (1.34 g, 27%).

1. temperatureThe reaction mixture is refluxed for 6 hours
2. extractionthe mixture is extracted with EtOAc (3×)
3. dry with materialThe organic layers are dried over MgSO4
4. filtrationfiltered
5. concentrationconcentrated
6. customThe crude product is purified by silica gel column chromatography
7. washeluting with 98:2 petroleum ether-EtOAc