تفاعل #2171030

معادلة التفاعل

potassium carbonate

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

phenyl boric acid

→

yellow product

المردود 81.8%

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

المردود 81.8%

المذيبات

water

1,2-dimethoxyethane

ظروف التفاعل

المعالجة

1. 1
   أخرىThe resulting reaction mixture
2. 2
   درجة الحرارةis subsequently heated
3. 3
   درجة الحرارةunder reflux under nitrogen
4. 4
   درجة الحرارةAfter five hours the reaction mixture is heated over silica gel (hyflo super-gel of Celite Co.)
5. 5
   ترشيحfiltered
6. 6
   درجة الحرارةthe filtrate cooled in an ice bath
7. 7
   ترشيحThe precipitate coming down is filtered
8. 8
   غسيلwashed with water
9. 9
   أخرىrecrystallized from 50 ml ethanol
10. 10
    أخرىAfter drying in vacuum at 60° C. one

الإجراء التجريبي

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.

المصدر