Reacción #2171030

Ecuación de reacción

potassium carbonate

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

phenyl boric acid

→

yellow product

Rendimiento 81.8%

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

Rendimiento 81.8%

Disolventes

water

1,2-dimethoxyethane

Condiciones de reacción

Tratamiento posterior

1. 1
   OtroThe resulting reaction mixture
2. 2
   Temperaturais subsequently heated
3. 3
   Temperaturaunder reflux under nitrogen
4. 4
   TemperaturaAfter five hours the reaction mixture is heated over silica gel (hyflo super-gel of Celite Co.)
5. 5
   Filtraciónfiltered
6. 6
   Temperaturathe filtrate cooled in an ice bath
7. 7
   FiltraciónThe precipitate coming down is filtered
8. 8
   Lavadowashed with water
9. 9
   Otrorecrystallized from 50 ml ethanol
10. 10
    OtroAfter drying in vacuum at 60° C. one

Procedimiento

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.

Fuente