反应详情

To a 0° C. solution of 1.4 M MeLi in Et2O (35 mm) was added 5-phenylpyridine (4.65 g). The Et2O was distilled off almost completely and replaced by THF (15 cc) and the solution was refluxed for 1 hour. 25% aqueous NH4OAc (25 cc) was added and the mixture extracted with ethyl acetate (2×50 cc). The organic layer was washed with brine and the solvents removed in vacuo. The residue was purified by chromatography to afford the title compound. p.m.r. (CD3COCD3) δ 8.7 (d, 1H), 7.2-7.9 (m, 7H), 2.5 (s, 3H).

1. distillationThe Et2O was distilled off almost completely
2. temperaturethe solution was refluxed for 1 hour
3. addition25% aqueous NH4OAc (25 cc) was added
4. extractionthe mixture extracted with ethyl acetate (2×50 cc)
5. washThe organic layer was washed with brine
6. customthe solvents removed in vacuo
7. customThe residue was purified by chromatography