反应详情

A mixture of 3.1 g (13.2 mM) of 2-iodo-5-methoxypyridine, 2.9 g (19.8 mM) of 4-cyanophenylboronic acid, 1.7 g (40 mM) of lithium chloride, 0.6 g (0.52 mM) of tetrakis(triphenylphosphine)palladium, 30 ml of methanol and 30 ml of toluene is prepared and 20 ml (40 mM) of 2 M sodium carbonate are added. The reaction mixture is heated at the reflux temperature of the solvent for 72 hours. The phases are separated and the aqueous phase is extracted with ethyl acetate. The combined organic phases are washed with N sodium hydroxide solution, with water and with saturated sodium chloride solution and then dried over magnesium sulfate. After evaporation of the solvents, the crude product is purified by chromatography on silica gel using dichloromethane as the eluent to give the expected product in the form of a pale yellow solid with a yield of 66%.

1. customis prepared
2. temperatureThe reaction mixture is heated at the reflux temperature of the solvent for 72 hours
3. customThe phases are separated
4. extractionthe aqueous phase is extracted with ethyl acetate
5. washThe combined organic phases are washed with N sodium hydroxide solution, with water and with saturated sodium chloride solution
6. dry with materialdried over magnesium sulfate
7. customAfter evaporation of the solvents
8. customthe crude product is purified by chromatography on silica gel