반응 #2171030

반응 방정식

potassium carbonate

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

phenyl boric acid

→

yellow product

수율 81.8%

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

수율 81.8%

용매

water

1,2-dimethoxyethane

반응 조건

후처리

1. 1
   기타The resulting reaction mixture
2. 2
   온도is subsequently heated
3. 3
   온도under reflux under nitrogen
4. 4
   온도After five hours the reaction mixture is heated over silica gel (hyflo super-gel of Celite Co.)
5. 5
   여과filtered
6. 6
   온도the filtrate cooled in an ice bath
7. 7
   여과The precipitate coming down is filtered
8. 8
   세척washed with water
9. 9
   기타recrystallized from 50 ml ethanol
10. 10
    기타After drying in vacuum at 60° C. one

실험 절차

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.

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