HRID1263569
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
6,6′-bis(2-Hydroxy-3-ethoxyphenyl)-2,2′-bipyridine was prepared by reaction of 2-hydroxy-3-ethoxyphenylboronic acid (836 mg, 4.60 mmol) with 6,6-dibromo-2,2′-bipyridyl (722 mg, 2.30 mmol), sodium carbonate (2N solution, 6ml) and tetrakis(triphenylphosphine) palladium (40 mg) in ethylene glycol dimethyl ether (30 ml) at reflux under nitrogen for 4 hours. The solid was filtered from the cooled reaction and washed with ether and water and toluene, to give the desired product as a yellow solid (446 mg, 48%); δH [2H6]-DMSO 8.33,(2H, d), 8.23,(2H, t), 8.14,(2H, d), 7.68,(2H, d), 7.05,(2H, d), 6.88,(2H, t), 4.06,(4H, q), 1.35,(6H, t).
WORKUP
后处理
- temperatureat reflux under nitrogen for 4 hours
- filtrationThe solid was filtered from the cooled reaction
- washwashed with ether and water and toluene