Reaktion #93663

Reaktionsgleichung

acetic anhydride

nitric acid

5-propionamido-1-(2,3,4-trichlorophenyl)-pyrazole

→

4-nitro-5-propionamido-1-(2,3,4-trichlorophenyl)-pyrazole

Ausbeute 76.0%

Lösungsmittel

acetic acid

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONWhen the addition
2. 2
   Sonstigeis evaporated down in vacuo
3. 3
   Waschenthe solution is washed three times with a total of 50 to 100 ml of concentrated sodium bicarbonate solution
4. 4
   Sonstigetwice with 50 ml of saturated sodium chloride solution, the solvent is removed in a vacuum from a water pump
5. 5
   Waschenthe solid residue is washed with a small amount of water
6. 6
   Sonstigedried in a high vacuum at 30° C. to 40° C

Vorschrift

2 ml (2.17 g/0.021 mol) of acetic anhydride and then 0.9 ml (1.3 g/0.02 mol) of 98% strength nitric acid are added in succession to 6.4 g (0.02 mol) of 5-propionamido-1-(2,3,4-trichlorophenyl)-pyrazole in 20 ml of glacial acetic acid at 10° C. When the addition is complete, the mixture is stirred for 16 hours at 25° C. To work up the mixture, it is evaporated down in vacuo, the residue is taken up in 20 ml of diethyl ether, the solution is washed three times with a total of 50 to 100 ml of concentrated sodium bicarbonate solution and twice with 50 ml of saturated sodium chloride solution, the solvent is removed in a vacuum from a water pump, and the solid residue is washed with a small amount of water and dried in a high vacuum at 30° C. to 40° C. 5.5 g (76% of theory) of 4-nitro-5-propionamido-1-(2,3,4-trichlorophenyl)-pyrazole of melting point 79°-81° C. are obtained.

Quelle