反应详情

温度

95 °C

32.4 g of 4′-iodobiphenyl-4-carboxylic acid are introduced together with 25.8 g of glycol ester of 4-n-pentoxyphenylboronic acid and 15.9 g of sodium carbonate into 300 ml of ethylene glycol and, while stirring vigorously, 70 mg of PdCl2(PPh3)2 are added, and the mixture is stirred at 120° C. for 6 hours. The hot reaction mixture is cautiously poured into a mixture of 30 g of 37% strength sulfuric acid and 200 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 25.2 g (70%) of 4″-n-pentoxy-[1,1′:4′,1″]-4-carboxylic acid with a purity of >99%.

1. stirringthe mixture is stirred at 120° C. for 6 hours
2. filtrationAfter filtration
3. washwashing with water
4. dry with materialthe crude product is dried at 80° C./100 mbar
5. customrecrystallized from dimethylacetamide
6. customThis affords
7. dry with materialafter drying 25.2 g (70%) of 4″-n-pentoxy-[1,1′:4′,1″]-4-carboxylic acid with a purity of >99%