反应详情

To a degassed solution of dimethyl 4-ethenyl-1,3-benzenedicarboxylate (415 mg, 1.88 mmol) in benzene (6 mL) were added AIBN (33 mg, 0.21 mmol) and thioacetic acid (0.27 mL, 3.78 mmol), and the mixture was refluxed for 5 hours. The reaction mixture was diluted with aqueous NaHCO3 solution (15 mL) and extracted with EtOAc (15 mL). The organic layer was dried over MgSO4 and concentrated. The residual material was purified by silica gel chromatography (hexanes/EtOAc=10:1) to give 0.150 g of colorless oil (27% yield).

1. temperaturethe mixture was refluxed for 5 hours
2. extractionextracted with EtOAc (15 mL)
3. dry with materialThe organic layer was dried over MgSO4
4. concentrationconcentrated
5. customThe residual material was purified by silica gel chromatography (hexanes/EtOAc=10:1)