反应详情

To a cooled (−70° C.) solution of 3-phenylpyridine (1.43 mL, 10.0 mmoles) in diethyl ether (7.5 mL) is added dropwise methyllithium (LiBr complex, 1.5 M in diethyl ether, 7.33 mL, 11.0 mmoles). After letting warm to room temperature over 16 hours the reaction is cooled (0° C.) and quenched with distilled water (5 mL). The reaction is then extracted with methylene chloride, the organic layer isolated and concentrated, and the resulting residue purified by column chromatography (silica, 3:1 hexane: EtOAc) to yield the title compound as a pale yellow oil. MS(ESI) 170 (M+H)+.

1. temperatureis cooled (0° C.)
2. customquenched with distilled water (5 mL)
3. extractionThe reaction is then extracted with methylene chloride
4. customthe organic layer isolated
5. concentrationconcentrated
6. customthe resulting residue purified by column chromatography (silica, 3:1 hexane: EtOAc)