Réaction #1287050

ord-1af89ec8c84142189f6929b5f1dcef71

Conditions de réaction

Température
-5°CELSIUS
Conditions détaillées
See reaction.notes.procedure_details.

Traitement

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

Mode opératoire

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° 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°-100° C.). It can optionally be recrystallized from 96° strength ethanol.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US04904276uspto-grants-1990_02