반응 #667151

반응 방정식

nitric acid

N-acetyl-2,6-xylidine

acetic acid

sulfuric acid

→

title compound

수율 94.7%

N-acetyl-2,6-dimethyl-3-nitroaniline

수율 94.7%

반응 조건

후처리

1. 1
   온도cooling
2. 2
   기타did not exceed 10° C
3. 3
   기타was returned to room temperature
4. 4
   workup.STIRRINGafter stirring for 2 hours
5. 5
   workup.ADDITIONpoured onto ice
6. 6
   여과The resulting crystalline precipitate was collected by filtration
7. 7
   기타recrystallized from ethanol

실험 절차

To a mixture of 30.1 g of N-acetyl-2,6-xylidine (0.18 mole) and 40 ml of acetic acid (0.70 mole) was added gradually 80 ml of concentrated sulfuric acid (0.50 mole) with stirring under ice-cooling. Then, to the mixture was added slowly 10 ml of fuming nitric acid (0.24 mole) in a manner such that the temperature of the reaction mixture did not exceed 10° C. The reaction mixture was returned to room temperature and, after stirring for 2 hours, poured onto ice. The resulting crystalline precipitate was collected by filtration and recrystallized from ethanol to give 35.5 g (92%) of the title compound (m.p. 171°-173° C.; pale yellow needles).

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