反应详情

bis(2-Hydroxy-3,5-dimethylphenyl)-2,2′-bipyridine was prepared by reaction of 2-hydroxy-3,5-dimethylphenylboronic acid (321 mg, 1.92 mmol) with 6,6-dibromo-2,2′-bipyridyl (260 mg, 0.82 mmol), sodium carbonate (2N solution, 2 ml) and tetrakis(triphenylphosphine) palladium (20 mg) in ethylene glycol dimethyl ether (8 ml) at reflux under nitrogen for 88 hours. The solid was filtered from the cooled reaction and washed with acetone and water to give the desired product as a yellow solid (220 mg, 68%); δH [2H6]-DMSO 8.39,(2H, d), 8.31,(2H, t), 8.10,(2H, d), 7.78,(2H, s), 7.10,(2H, s), 2.31,(6H, s), 2.24,(6H, s).

1. temperatureat reflux under nitrogen for 88 hours
2. filtrationThe solid was filtered from the cooled reaction
3. washwashed with acetone and water