Hydrazine hydrate (1:1) → HCID 20096580, Verbindung

HRID 1769975Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1769975
O.NN.[CH2:4]([O:6][C:7]([NH:9][C:10]1[CH:15]=[CH:14][C:13]([N:16]2C(=O)C3=CC=CC=C3C2=O)=[CH:12][C:11]=1[N+:27]([O-:29])=[O:28])=[O:8])[CH3:5]>COCCOC>[NH2:16][C:13]1[CH:14]=[CH:15][C:10]([NH:9][C:7]([O:6][CH2:4][CH3:5])=[O:8])=[C:11]([N+:27]([O-:29])=[O:28])[CH:12]=1

Komponenten

4

Edukt 2

HCID 24654Hydrazine hydrate (1:1)HCID 20096586HCID 20096586, Verbindung

Produkt 1

HCID 20096580HCID 20096580, VerbindungAusbeute 93,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 80711,2-DimethoxyethaneLösungsmittel

Versuchsvorschrift

21.0 g (0.42 mol) hydrazine hydrate is added dropwise with stirring under reflux to a suspension of 142.1 g (0.4 mol) 2-ethoxycarbonylamino-5-phthalimido-nitrobenzene in 700 ml 1,2-dimethoxyethane and the mixture is allowed to react for a further 2 hours. After cooling to room temperature, precipitated phthalyl hydrazide is filtered off and the dark red filtrate in the vacuum is evaporated to dryness. The remaining solid residue is recrystallized from about 150 ml toluene. 84.4 g 5-amino-2-ethoxycarbonylaminonitrobenzene are obtained as dark red crystals.

Aufarbeitung

  1. customto react for a further 2 hours
  2. customprecipitated phthalyl hydrazide
  3. filtrationis filtered off
  4. customthe dark red filtrate in the vacuum is evaporated to dryness
  5. customThe remaining solid residue is recrystallized from about 150 ml toluene

Quellen und Nachweise

ORD-Eintrag
ord-45b80b347353493b8e33c6cd48395418
Quelldatensatz
uspto-grants-1995_01
Patentnummer
US05384330

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