反応 #2171030

反応方程式

potassium carbonate

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

phenyl boric acid

→

yellow product

収率 81.8%

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

収率 81.8%

溶媒

water

1,2-dimethoxyethane

反応条件

後処理

1. 1
   その他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
   ろ過filtered
6. 6
   温度the filtrate cooled in an ice bath
7. 7
   ろ過The precipitate coming down is filtered
8. 8
   洗浄washed with water
9. 9
   その他recrystallized from 50 ml ethanol
10. 10
    その他After drying in vacuum at 60° C. one

実験手順

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.

出典