反应详情

温度

80 °C

To a solution of 3,4-dimethoxythiophenol (5.0 g, 29.4 mmol) in dry DMF (150 ml), were added chloroacetonitrile (1.85 ml, 29.4 mmol), anhydrous K2CO3 (6.09 g, 44.1 mmol) and DMAP (358 mg, 2.9 mmol). The reaction mixture was stirred at 80° C. for 20 h under nitrogen. After cooling, the mixture was filtered and concentrated in vacuo. The residue was combined with H2O, extracted with CH2Cl2, the combined organic phases were dried over anhydrous MgSO4, filtered and concentrated to give a crude oil. Flash chromatography (AcOEt) gave the title product (5.16 g, 84%).

1. temperatureAfter cooling
2. filtrationthe mixture was filtered
3. concentrationconcentrated in vacuo
4. extractionextracted with CH2Cl2
5. dry with materialthe combined organic phases were dried over anhydrous MgSO4
6. filtrationfiltered
7. concentrationconcentrated
8. customto give a crude oil