HRID369628

反应详情

EQUATION

反应方程式

HRID 369628 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

PROCEDURE

实验过程

15 g of 2-chlorobenzonitrile, 15.8 g of p-tolueneboronic acid and 15.8 g of potassium fluoride in 50 ml of p-xylene, 40 ml of glycol and 10 ml of water were heated to 120° C. At 80° C., a mixture of 24.7 mg of palladium acetate and 0.55 ml of TPPTS/H2O solution (0.6 molar) in 2.5 ml of DMSO was added. After the reaction was complete, the phases were separated. The aqueous phase was washed with 50 ml of toluene. The combined organic phases were washed with 20 ml of water and subsequently dried over sodium sulfate. Crystallization from n-heptane gave 18.7 g of 2-cyano-4'-methylbiphenyl.

WORKUP

后处理

  1. additionwas added
  2. customthe phases were separated
  3. washThe aqueous phase was washed with 50 ml of toluene
  4. washThe combined organic phases were washed with 20 ml of water
  5. dry with materialsubsequently dried over sodium sulfate
  6. customCrystallization from n-heptane