反应 #2171030

反应方程式

potassium carbonate

1,3-bis-(5-benzylamino-3-bromo-4-nitropyrazol-1-yl)propane

phenyl boric acid

→

yellow product

收率 81.8%

1,3-bis-(5-benzylamino-4-nitro-3-phenyl-pyrazol-1-yl)propane

收率 81.8%

溶剂

water

1,2-dimethoxyethane

反应条件

后处理

1. 1
   其他The resulting reaction mixture
2. 2
   温度is subsequently heated
3. 3
   温度under reflux under nitrogen
4. 4
   温度After five hours the reaction mixture is heated over silica gel (hyflo super-gel of Celite Co.)
5. 5
   过滤filtered
6. 6
   温度the filtrate cooled in an ice bath
7. 7
   过滤The precipitate coming down is filtered
8. 8
   洗涤washed with water
9. 9
   其他recrystallized from 50 ml ethanol
10. 10
    其他After drying in vacuum at 60° C. one

实验过程

3.7 g of 1,3-bis-(5-benzylamino-3-bromo-4-nitropyrazol-1-yl)propane from step 5.2 in 40 ml 1,2-dimethoxyethane are mixed under nitrogen with 3.8 g phenyl boric acid, 1.2 g of tetrakis(triphenylphosphin)palladium (0) and a solution of 8.3 g of potassium carbonate in 30 ml water. The resulting reaction mixture is subsequently heated under reflux under nitrogen. After five hours the reaction mixture is heated over silica gel (hyflo super-gel of Celite Co.), filtered and the filtrate cooled in an ice bath. The precipitate coming down is filtered, washed with water and recrystallized from 50 ml ethanol. After drying in vacuum at 60° C. one obtains 1.5 g of a yellow product.

来源