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
CONDITIONS
反应条件
- 温度
- 95 °C
PROCEDURE
实验过程
162 g of 4′-iodobiphenyl-4-carboxylic acid are introduced together with 129 g of glycol ester of 4-n-pentoxyphenylboronic acid and 79.5 g of sodium carbonate into 1.5 l of ethylene glycol and, while stirring vigorously, 350 mg of PdCl2(PPh3)2 are added and the mixture is stirred at 80° C. for 6 hours. The hot reaction mixture is cautiously poured into a mixture of 150 g of 37% strength sulfuric acid and 1,000 g of water, and the mixture is heated at 90-100° C. for 30 minutes. After filtration and washing with water, the crude product is dried at 80° C./100 mbar and then recrystallized from dimethylacetamide. This affords after drying 141 g (78%) of 4″-n-pentoxy-[1,1′:4′,1″]-terphenyl-4-carboxylic acid with a purity of >99%.
WORKUP
后处理
- stirringthe mixture is stirred at 80° C. for 6 hours
- filtrationAfter filtration
- washwashing with water
- dry with materialthe crude product is dried at 80° C./100 mbar
- customrecrystallized from dimethylacetamide
- customThis affords
- dry with materialafter drying 141 g (78%) of 4″-n-pentoxy-[1,1′:4′,1″]-terphenyl-4-carboxylic acid with a purity of >99%