反应详情

温度

80 °C

To a stirred mixture of 3-methoxyphenol (200 mg, 1.61 mmol) in MeCN (5 mL) was added ethyl bromoacetate (402 mg, 2.42 mmol) and K2CO3 (672 mg, 4.83 mmol). The mixture was stirred at 80° C. for 4 hours, filtered and the filtrate concentrated. NaOH (129 mg, 3.22 mmol) and H2O/EtOH (1:1, 10 mL) was added to the mixture. The reaction mixture was stirred at 50° C. for 4 hours then acidified by 1M HCl and then extracted with ethyl acetate (2×30 mL). The combined organic extracts were washed with brine (30 mL), dried over anhydrous Na2SO4 and concentrated with the residue used directly for the next step. LCMS (m/z): 183.0 (M+1).

1. filtrationfiltered
2. concentrationthe filtrate concentrated
3. stirringThe reaction mixture was stirred at 50° C. for 4 hours
4. extractionextracted with ethyl acetate (2×30 mL)
5. washThe combined organic extracts were washed with brine (30 mL)
6. dry with materialdried over anhydrous Na2SO4
7. concentrationconcentrated with the residue