反应详情

温度

100 °C

A mixture of 4-(methylthio)phenylacetic acid (5.10 g, 28.0 mmol) and H2SO4 (0.155 mL, 2.80 mmol) in EtOH (150 mL) in a 500 mL round bottom flask, were stirred at 100° C. for 26 hours. The reaction was concentrated in vacuo, diluted with EtOAc (200 mL), washed with deionized water (2×150 mL), and then with brine (100 mL). The organic layer was dried over MgSO4, concentrated, and dried in vacuo. The crude product was purified by flash column chromatography (silica, 0-20% EtOAc in hexane) to give the title compound (5.95 g). MS m/e=211 (M+H)+.

1. concentrationThe reaction was concentrated in vacuo
2. additiondiluted with EtOAc (200 mL)
3. washwashed with deionized water (2×150 mL)
4. dry with materialThe organic layer was dried over MgSO4
5. concentrationconcentrated
6. customdried in vacuo
7. customThe crude product was purified by flash column chromatography (silica, 0-20% EtOAc in hexane)