Reaktion #955959

ord-f11756a4981b49de9f72b0641e8e7f9d

Reaktionsgleichung

CCCCC(CC)COc1cc([N+](=O)[O-])c([N+](=O)[O-])cc1OCC(CC)CCCC
1,2-bis((2-ethylhexyl)oxy)-4,5-dinitrobenzene
NN.O
hydrazine monohydrate
CCCCC(CC)COc1cc(N)c(N)cc1OCC(CC)CCCC
product
CCCCC(CC)COc1cc(N)c(N)cc1OCC(CC)CCCC
4,5-bis((2-ethylhexyl)oxy)benzene-1,2-diamine

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeA 250 mL 3-neck round bottom flask fitted with a condenser
  2. 2
    TemperaturThe mixture is warmed
  3. 3
    Temperaturto reflux under nitrogen overnight
  4. 4
    FiltrationThe mixture is filtered while hot under a nitrogen blanket
  5. 5
    SonstigeA solid is precipitated out
  6. 6
    Temperaturupon cooling
  7. 7
    Waschenwashed with methanol
  8. 8
    Sonstigedried overnight under vacuum

Vorschrift

A 250 mL 3-neck round bottom flask fitted with a condenser is charged with 1,2-bis((2-ethylhexyl)oxy)-4,5-dinitrobenzene (8.9 g, 0.021 mol), hydrazine monohydrate (11.6 g, 0.231 mol), Pd/C (0.27 g), and ethanol (100 mL). The mixture is warmed to reflux under nitrogen overnight. The mixture is filtered while hot under a nitrogen blanket. A solid is precipitated out upon cooling, washed with methanol and dried overnight under vacuum to yield the product as a white solid.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08968885B2uspto-grants-2015_03