Water → HCID 20301865, Verbindung

HRID 1732869Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1732869
[Cl:1][C:2]1[C:8](Cl)=[C:7]([N+:10]([O-:12])=[O:11])[CH:6]=[CH:5][C:3]=1[NH2:4].[CH3:13][O-:14].[Na+].O>CO>[Cl:1][C:2]1[C:8]([O:14][CH3:13])=[C:7]([N+:10]([O-:12])=[O:11])[CH:6]=[CH:5][C:3]=1[NH2:4]

Komponenten

5

Edukt 3

HCID 962WaterHCID 30139982,3-dichloro-4-nitroanilineHCID 10942334Sodium Methoxide

Produkt 1

HCID 20301865HCID 20301865, VerbindungAusbeute 53,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

A solution of 2,3-dichloro-4-nitroaniline (25 g) and sodium methoxide (25 g) in methanol (250 ml) is stirred and heated at reflux under a nitrogen atmosphere for 5.5 hours. The reaction mixture is poured into water (1.5 l), the precipitated yellow solid is collected and dried. This material is purified by chromatography on silica gel using 1:1 hexane/ether eluent. The eluents are collected and evaporated to dryness to afford 13 g of title compound, m.p. 118°-123° C.

Aufarbeitung

  1. temperatureheated
  2. temperatureat reflux under a nitrogen atmosphere for 5.5 hours
  3. customthe precipitated yellow solid is collected
  4. customdried
  5. customThis material is purified by chromatography on silica gel using 1:1 hexane/ether eluent
  6. customThe eluents are collected
  7. customevaporated to dryness

Quellen und Nachweise

ORD-Eintrag
ord-6421c56451444848914f136bc6cca713
Quelldatensatz
uspto-grants-1980_12
Patentnummer
US04239708

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