Reaktion #2171030

Reaktionsgleichung

potassium carbonate

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

phenyl boric acid

→

yellow product

Ausbeute 81.8%

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

Ausbeute 81.8%

Lösungsmittel

water

1,2-dimethoxyethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe resulting reaction mixture
2. 2
   Temperaturis subsequently heated
3. 3
   Temperaturunder reflux under nitrogen
4. 4
   TemperaturAfter five hours the reaction mixture is heated over silica gel (hyflo super-gel of Celite Co.)
5. 5
   Filtrationfiltered
6. 6
   Temperaturthe filtrate cooled in an ice bath
7. 7
   FiltrationThe precipitate coming down is filtered
8. 8
   Waschenwashed with water
9. 9
   Sonstigerecrystallized from 50 ml ethanol
10. 10
    SonstigeAfter drying in vacuum at 60° C. one

Vorschrift

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.

Quelle