反应 #417985

反应方程式

tert-butyl methyl ether

5-bromo-2-iodo-pyrimidine

tripotassium phosphate trihydrate

3-(hydroxymethyl)benzeneboronic acid

→

[3-(5-bromopyrimidin-2-yl)phenyl]methanol

溶剂

water

dioxane

water

反应条件

后处理

1. 1
   温度The reaction mixture is cooled to room temperature
2. 2
   过滤the mixture is filtered through kieselguhr
3. 3
   其他The organic phase of the filtrate is separated off
4. 4
   干燥dried over sodium sulfate
5. 5
   其他evaporated
6. 6
   其他The residue is chromatographed on a silica-gel column with dichloromethane/methanol as eluent

实验过程

750 mg (0.65 mmol) of tetrakis(triphenylphosphine)palladium are added to a solution, kept under nitrogen, of 6.11 g (21.5 mmol) of 5-bromo-2-iodo-pyrimidine, 3.91 g (25.7 mmol) of 3-(hydroxymethyl)benzeneboronic acid and 9.11 g (42.9 mmol) of tripotassium phosphate trihydrate in 120 ml of dioxane and 14 ml of water, and the mixture is stirred at 90° C. for 18 hours. The reaction mixture is cooled to room temperature, tert-butyl methyl ether and water are added, and the mixture is filtered through kieselguhr. The organic phase of the filtrate is separated off, dried over sodium sulfate and evaporated. The residue is chromatographed on a silica-gel column with dichloromethane/methanol as eluent; product: 2.49 g;

来源