Ethanol → HCID 178433518, Verbindung

HRID 544743Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 544743
[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[NH:7][NH:8][C:9]([NH2:11])=[O:10].[CH2:12](O)[CH3:13]>C(C(CC)(CC)C([O-])([O-])[O-])C>[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[N:7]1[C:12]([CH3:13])=[N:11][C:9]([OH:10])=[N:8]1

Komponenten

4

Edukt 2

HCID 702EthanolHCID 13366065Hydrazinecarboxamide, 2-(2-pyridinyl)-

Produkt 1

HCID 178433518HCID 178433518, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 21875354TriethylorthoaceateLösungsmittel

Versuchsvorschrift

A reaction mixture was prepared by suspending 457.6 g (3 m) of 2-pyridinyl-hydrazine carboxamide in 2600 ml of triethylorthoacetate and the mixture refluxed for about 9 hours. The ethanol by-product formed was continuously removed by distillation allowing the reaction temperature to stay at 125°-130° C. The 1-(2-pyridinyl)-5-methyl-1H-1,2,4-triazol-3-ol product was recovered by filtration in a yield of 116 g (66 percent of theoretical) and was washed with chloroform. The product melted at 194°-195° C. and upon analysis was found to have carbon hydrogen and nitrogen contents of 53.87, 4.55 and 31.95 percent, respectively, as compared with the theoretical contents of 54.53, 4.57 and 31.80 percent, respectively, calculated for the above named compound.

Aufarbeitung

  1. customA reaction mixture was prepared
  2. temperaturethe mixture refluxed for about 9 hours
  3. customwas continuously removed by distillation
  4. customto stay at 125°-130° C
  5. filtrationThe 1-(2-pyridinyl)-5-methyl-1H-1,2,4-triazol-3-ol product was recovered by filtration in a yield of 116 g (66 percent of theoretical)
  6. washwas washed with chloroform

Quellen und Nachweise

ORD-Eintrag
ord-2555864375af478ab532216030b41189
Quelldatensatz
uspto-grants-1984_05
Patentnummer
US04451653

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