Reaktion #666870

ord-0e8e693e1afa4941b8829c7dfb596853

Reaktionsgleichung

O=[N+]([O-])c1cc2c(cc1[N+](=O)[O-])OCO2
4,5-methylenedioxy-1,2-dinitrobenzene
CN
methylamine
CNc1cc2c(cc1[N+](=O)[O-])OCO2
2-methylamino-4,5-methylenedioxy-1-nitrobenzene

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONhave been added
  2. 2
    TemperaturThe reaction edium is heated
  3. 3
    Temperaturunder reflux for 30 minutes
  4. 4
    SonstigeAfter dilution with 150 ml of ice-cold water, the expected product precipitates
  5. 5
    Waschenwashed with water, it
  6. 6
    Sonstigeis recrystallized from a mixture of ethanol and acetone
  7. 7
    SonstigeIt melts at 170° C. (literature 171° C.)

Vorschrift

0.05 mol (10.6 g) of 4,5-methylenedioxy-1,2-dinitrobenzene is added to 40 ml of a 33% strength solution of methylamine in absolute ethanol to which 20 ml of 96° strength ethanol have been added. The reaction edium is heated under reflux for 30 minutes. After dilution with 150 ml of ice-cold water, the expected product precipitates. After being drained and washed with water, it is recrystallized from a mixture of ethanol and acetone. It melts at 170° C. (literature 171° C.).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04749379uspto-grants-1988_06