Hydrazine → HCID 178465624, Verbindung

HRID 1720215Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1720215
I.CS[C:4](=[NH:13])[NH:5][C:6]1[CH:11]=[CH:10][CH:9]=[C:8]([F:12])[CH:7]=1.[NH2:14][NH2:15].[C:16]([C:19]1[N:27]=[CH:26][CH:25]=[CH:24][C:20]=1[C:21]([OH:23])=[O:22])(=O)[CH3:17]>C(O)C.CO>[CH3:17][C:16]([C:19]1[C:20]([C:21]([OH:23])=[O:22])=[CH:24][CH:25]=[CH:26][N:27]=1)=[N:14][NH:15][C:4](=[NH:13])[NH:5][C:6]1[CH:11]=[CH:10][CH:9]=[C:8]([F:12])[CH:7]=1

Komponenten

6

Edukt 3

HCID 9321HydrazineHCID 101762782-Acetyl-3-pyridinecarboxylic acidHCID 178503998HCID 178503998, Verbindung

Produkt 1

HCID 178465624HCID 178465624, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittelHCID 887MethanolLösungsmittel

Versuchsvorschrift

A mixture of the above isothiourea salt (8.5 g, 27.0 mmol) and hydrazine (1.4 g, 27.0 mmol) in 80 ml of ethanol is heated to reflux for 4 hr. The mixture is cooled and the solvent removed. The residue is diluted with 80 ml of water and filtered. A 20 ml aliquot of the resulting aqueous filtrate (2.0 g, 11.9 mmol) is mixed with 2-acetylnicotinic acid (2.0 g, 11.9 mmol) in 6 ml of methanol and stirred at RT overnight. A bright yellow solid is collected by filtration and dried to give 2-[methyl(3-carboxy-2-pyridyl)methylene]-N-(3-fluorophenyl)hydrazinecarboximidamide, (compound 16).

Aufarbeitung

  1. temperatureis heated
  2. temperatureto reflux for 4 hr
  3. temperatureThe mixture is cooled
  4. customthe solvent removed
  5. additionThe residue is diluted with 80 ml of water
  6. filtrationfiltered
  7. filtrationA bright yellow solid is collected by filtration
  8. customdried

Quellen und Nachweise

ORD-Eintrag
ord-e6dd7eccb4f04dd4a7a067fa5265619c
Quelldatensatz
uspto-grants-1996_04
Patentnummer
US05506191

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