反应详情

温度

22 °C

To an acetone solution containing pulverized anhydrous K2CO3 (5.58 g, 40.5 mmol) and 2-bromophenol (5.0 g, 28.9 mmol) was added ethyl 4-bromocrotonate (6.69 g, 34.7 mmol). The mixture was stirred at 22° C. for 5 h and filtered. The filtrate was concentrated in vacuo and treated with 5% NaHCO3 (~10 mL). The residue and aqueous phase were extracted with CH2Cl2 (3×). The combined organic extracts were dried with anhydrous MgSO4, filtered, and concentrated in vacuo to afford the title compound (6.10 g, 74%) as a solid material which was used without further purification.

1. filtrationfiltered
2. concentrationThe filtrate was concentrated in vacuo
3. additiontreated with 5% NaHCO3 (~10 mL)
4. extractionThe residue and aqueous phase were extracted with CH2Cl2 (3×)
5. dry with materialThe combined organic extracts were dried with anhydrous MgSO4
6. filtrationfiltered
7. concentrationconcentrated in vacuo