反应详情

A mixture of 2-fluoro-6-methoxybenzonitrile (15.94 g, 105.5 mmol) and a solution of methyl magnesium iodide in diethyl ether (3 M, 46.0 cm3, 137 mmol) was heated to 100° C. for 18 h. Upon cooling to room temperature, aqueous hydrochloric acid (3 M, 94 cm3) was added and the mixture was heated to reflux to for 4 h. When the reaction had cooled to room temperature the organic layer was separated and the aqueous phase was extracted with ethyl acetate (100 cm3). The combined organic extracts were washed with brine (100 cm3) before being dried (Na2SO4). The solvent was removed in vacuo to afford the title compound as an oil (117.7 g, 100%).

1. temperaturethe mixture was heated
2. temperatureto reflux to for 4 h
3. temperatureWhen the reaction had cooled to room temperature the organic layer
4. customwas separated
5. extractionthe aqueous phase was extracted with ethyl acetate (100 cm3)
6. washThe combined organic extracts were washed with brine (100 cm3)
7. dry with materialbefore being dried (Na2SO4)
8. customThe solvent was removed in vacuo