HRID1884207

反应详情

EQUATION

反应方程式

HRID 1884207 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

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

  1. stirringthe mixture is stirred at 80° 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 141 g (78%) of 4″-n-pentoxy-[1,1′:4′,1″]-terphenyl-4-carboxylic acid with a purity of >99%