反应详情

温度

80 °C

To a solution of 3-amino-2-fluorobenzoic acid (500 mg, 3.1 mmol) in DMF (10 mL) was added DIEA (4.5 mL) and 2-bromoethylether (5 eq) and the reaction heated to 80° C. for 18 h. The reaction was allowed to cool to rt, diluted with EtOAc and washed with saturated NH4Cl (aq). The organic phase was dried (Na2SO4), filtered and concentrated in vacuo. The resultant residue was purified by column chromatography (petroleum ether: EtOAc) to give 2-(2-bromoethoxy)ethyl 2-fluoro-3-morpholinobenzoate (450 mg, 38%) as a yellow oil.

1. temperatureto cool to rt
2. washwashed with saturated NH4Cl (aq)
3. dry with materialThe organic phase was dried (Na2SO4)
4. filtrationfiltered
5. concentrationconcentrated in vacuo
6. customThe resultant residue was purified by column chromatography (petroleum ether: EtOAc)