반응 #736832

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4,5-methylenedioxy-1-nitrobenzene

nitric acid

nitric acid

→

4,5-methylenedioxy-1,2-dinitrobenzene

반응 조건

후처리

1. 1
   온도the temperature being maintained at between 0° C. and 5° C
2. 2
   workup.ADDITION1 hour after the addition
3. 3
   기타the expected product precipitates
4. 4
   건조After being dried hot in the presence of phosphorus pentoxide, it melts at 99° C. (literature 98° C.-100° C.)
5. 5
   기타It can optionally be recrystallized from 96° strength ethanol

실험 절차

0.103 mol (17.2 g) of 4,5-methylenedioxy-1-nitrobenzene is added in small portions in the course of 15 minutes to a mixture, cooled to -5° C., consisting of 125 ml of nitric acid (d=1.50) and 125 ml of nitric acid (d=1.40), the temperature being maintained at between 0° C. and 5° C. 1 hour after the addition is complete, the reaction mixture is poured onto 1 kg of ice; the expected product precipitates. After being dried hot in the presence of phosphorus pentoxide, it melts at 99° C. (literature 98° C.-100° C.). It can optionally be recrystallized from 96° strength ethanol.

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