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Hydrazinecarboxaldehyde → 3-(4-nitrophenyl)-1H-1,2,4-triazole

HRID 1807198
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Reaktionsgleichung

Reaktionsgleichung von HRID 1807198
Cl.CO[C:4](=[NH:14])[C:5]1[CH:10]=[CH:9][C:8]([N+:11]([O-:13])=[O:12])=[CH:7][CH:6]=1.[CH:15]([NH:17][NH2:18])=O>N1C=CC=CC=1>[N+:11]([C:8]1[CH:7]=[CH:6][C:5]([C:4]2[NH:18][N:17]=[CH:15][N:14]=2)=[CH:10][CH:9]=1)([O-:13])=[O:12]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 12229HydrazinecarboxaldehydeHCID 12410479HCID 12410479, Verbindung

Produkt 1

HCID 28252243-(4-nitrophenyl)-1H-1,2,4-triazole

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1049PyridineLösungsmittel

Versuchsvorschrift

4-Nitro-benzimidic acid methyl ester hydrochloride (635 mg, 2.93 mmol) was suspended in pyridine (7 mL) and formic hydrazide (Aldrich, 178 mg, 2.95 mmol) was added and the mixture was stirred at rt for 1 hr. The solvent was removed and the residue was dissolved in toluene (10 mL) and the mixture was stirred at reflux for 1.5 hrs. the mixture was cooled and water was added. The organic layer was separated and dried over sodium sulfate. The solvent was removed and the residue was suspended in 25% EtOAc/Hexanes and the solid was filtered to give a solid. 510 mg.

Aufarbeitung

  1. customThe solvent was removed
  2. dissolutionthe residue was dissolved in toluene (10 mL)
  3. stirringthe mixture was stirred
  4. temperatureat reflux for 1.5 hrs
  5. temperaturethe mixture was cooled
  6. additionwater was added
  7. customThe organic layer was separated
  8. dry with materialdried over sodium sulfate
  9. customThe solvent was removed
  10. filtrationthe solid was filtered
  11. customto give a solid

Quellen und Nachweise

ORD-Eintrag
ord-e9d962c9286948cbac36aa0a6d7abc96
Quelldatensatz
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08354444B2

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