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Ammonium Chloride → HCID 13750559, Verbindung

HRID 1445476
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1445476
[CH3:1][O:2][C:3]1[CH:12]=[N:11][C:10]2[C:5](=[CH:6][CH:7]=[C:8]([N+:13]([O-])=O)[CH:9]=2)[N:4]=1.[Cl-].[NH4+]>[Fe].CO>[CH3:1][O:2][C:3]1[CH:12]=[N:11][C:10]2[C:5](=[CH:6][CH:7]=[C:8]([NH2:13])[CH:9]=2)[N:4]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 2

HCID 25517Ammonium ChlorideHCID 150258562-Methoxy-6-nitroquinoxaline

Produkt 1

HCID 13750559HCID 13750559, VerbindungAusbeute 124,2 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23925IronKatalysatorHCID 887MethanolLösungsmittel

Versuchsvorschrift

Into 20 ml of methanol was dissolved 726 mg of 2-methoxy-6-nitroquinoxaline, and then 1.0 g of iron powder and a saturated ammonium chloride aqueous solution were added thereto, followed by heating under refluxing overnight. Insoluble matter was separated by filtration using celite and then the solvent was removed by evaporation. A sodium bicarbonate aqueous solution was added to the residue, followed by extraction with ethyl acetate. After the organic layer was dried over anhydrous magnesium sulfate, the solvent was removed by evaporation and the resulting residue was purified by silica gel column chromatography to obtain 770 mg of the title compound from chloroform-methanol (100:1, v/v).

Aufarbeitung

  1. temperatureby heating
  2. temperatureunder refluxing overnight
  3. customInsoluble matter was separated by filtration
  4. customthe solvent was removed by evaporation
  5. additionA sodium bicarbonate aqueous solution was added to the residue
  6. extractionfollowed by extraction with ethyl acetate
  7. dry with materialAfter the organic layer was dried over anhydrous magnesium sulfate
  8. customthe solvent was removed by evaporation
  9. customthe resulting residue was purified by silica gel column chromatography

Quellen und Nachweise

ORD-Eintrag
ord-f6632d67e2df49c9be604e13f4098eb3
Quelldatensatz
uspto-grants-2010_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07666873B2

Notizen zur Reaktion

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