反应详情

To a flask containing methyl magnesium bromide (1.18 g, 9.93 mmol) in ether is added dropwise 2-fluoro-6-methoxybenzonitrile (0.5 g, 3.31 mmol, Lancaster Synthesis Inc.) in benzene (9 ml). The reaction mixture is refluxed overnight. The reaction is cooled to room temperature and quenched slowly with saturated ammonium chloride (15 ml) and concentrated hydrochloric acid (1 ml). The mixture is extracted with diethyl ether (2×50 ml). The combined organic layers are dried over Na2SO4, filtered, and rotary evaporated to give 0.55 g of a crude yellow material. Purification is accomplished by vacuum column (eluting with 16% ethyl acetate in hexane). The compoundcontaining fractions are combined, yielding 5.

1. temperatureThe reaction mixture is refluxed overnight
2. customquenched slowly with saturated ammonium chloride (15 ml) and concentrated hydrochloric acid (1 ml)
3. extractionThe mixture is extracted with diethyl ether (2×50 ml)
4. dry with materialThe combined organic layers are dried over Na2SO4
5. filtrationfiltered
6. customrotary evaporated
7. customto give 0.55 g of a crude yellow material
8. customPurification
9. washis accomplished by vacuum column (eluting with 16% ethyl acetate in hexane)
10. customyielding 5