HRID1642788

反应详情

EQUATION

反应方程式

HRID 1642788 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

CONDITIONS

反应条件

温度
85 °C

PROCEDURE

实验过程

4.68 g (20.32 mmol) of ethyl 5-bromonicotinate, 5.00 g (30.49 mmol) of 4-(1-methylethyl)-phenylboronic acid, 0.12 g (0.10 mmol) of tetrakis(triphenylphosphine)palladium(0) and 4.31 g (40.65 mmol) of sodium carbonate were dissolved in a mixture of 37 ml of 1,2-dimethoxyethane, 10.5 ml of water and 84 ml of dimethylformamide and stirred at 85° C. for 18 h. For work-up, some of the dimethylformamide was removed under reduced pressure, and the reaction mixture was diluted with water and extracted with dichloromethane. The organic phase was dried over sodium sulphate and the crude product was purified by preparative HPLC. Yield: 2.42 g (44% of theory)

WORKUP

后处理

  1. customFor work-up, some of the dimethylformamide was removed under reduced pressure
  2. additionthe reaction mixture was diluted with water
  3. extractionextracted with dichloromethane
  4. dry with materialThe organic phase was dried over sodium sulphate
  5. customthe crude product was purified by preparative HPLC