Reaktion #1062942

Reaktionsgleichung

Nitric acid

1-(2-chloro-4-fluorophenyl)-3-methyl-s-triazine-2,4,6(1H,3H,5H)-trione

→

title product

Ausbeute 75.6%

1-(2-Chloro-4-fluoro-5-nitrophenyl)-3-methyl-s-triazine-2,4,6(1H,3H,5H)-trione

Ausbeute 75.6%

Lösungsmittel

—

ice water

sulfuric acid

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwhile maintaining the reaction mixture temperature below 10° C
2. 2
   workup.ADDITIONAfter the addition
3. 3
   Temperaturcooled to 10° C.
4. 4
   FiltrationThe resultant aqueous mixture is filtered
5. 5
   Sonstigeto obtain a solid which
6. 6
   Waschenis washed with water
7. 7
   Sonstigeair-dried

Vorschrift

Nitric acid (70% real, 8.3 mL, 0.131 mol) is added to a solution of 1-(2-chloro-4-fluorophenyl)-3-methyl-s-triazine-2,4,6(1H,3H,5H)-trione (32.4 g, 0.119 mol) in concentrated sulfuric acid while maintaining the reaction mixture temperature below 10° C. After the addition is complete, the reaction mixture is stirred at room temperature for 30 minutes, cooled to 10° C. and diluted with ice-water. The resultant aqueous mixture is filtered to obtain a solid which is washed with water and air-dried to give the title product as a white solid (28.5 g, mp 135°-139° C.).

Quelle