反应详情

To a solution of 3-fluorophenol (1.2 g, 11.8 mmol) in 20 mL of DMF at 0° C. is added sodium hydride (0.47 g, 10.7 mmol). After stirring for 10 minutes Ethyl bromoacetate (1.2 g, 10.7 mmol) is added dropwise. The reaction is allowed to warm to ambient temperatures and is stirred for 16 hours. To the reaction is added a saturated solution NH4Cl (aq.). The resulting mixture is diluted with EtOAc and H2O. The layers are separted. The organic layer is washed with H2O and a saturated solution NaCl (aq.). The organic layer is dried over MgSO4, filtered and concentrated to give the product (2 g, 10 mmol) as an oil. 1H NMR (CDCl3, 300 MHz) δ7.22 (m, 1H), 6.65 (m, 3H), 4.61 (s, 2H), 4.27 (q, 2H), 1.24 (t, 3H).

1. additionis added dropwise
2. temperatureto warm to ambient temperatures
3. washThe organic layer is washed with H2O
4. dry with materialThe organic layer is dried over MgSO4
5. filtrationfiltered
6. concentrationconcentrated