[(6-Fluoropyridin-2-yl)amino]urea → HCID 178433516, Verbindung

HRID 544742Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 544742
[F:1][C:2]1[N:7]=[C:6]([NH:8][NH:9][C:10]([NH2:12])=[O:11])[CH:5]=[CH:4][CH:3]=1.[CH2:13](C(CC)(CC)C([O-])([O-])[O-])[CH3:14]>>[F:1][C:2]1[N:7]=[C:6]([N:8]2[C:13]([CH3:14])=[N:12][C:10]([OH:11])=[N:9]2)[CH:5]=[CH:4][CH:3]=1

Komponenten

3

Edukt 2

HCID 1478413[(6-Fluoropyridin-2-yl)amino]ureaHCID 21875354Triethylorthoaceate

Produkt 1

HCID 178433516HCID 178433516, VerbindungAusbeute 58,7 %

Versuchsvorschrift

A solution was prepared by admixing 17.02 g (0.10 m) of 2-(6-fluoro-2-pyridinyl)hydrazinecarboxamide with 100 ml of triethylorthoacetate. The mixture was refluxed overnight and the reaction mixture cooled to room temperature and poured over ice water. The solids which precipitated out were recovered by filtration. The solids were washed with methylene chloride and dried under vacuum to yield 11.4 g (58.7 percent of theoretical) of the desired 1-(6-fluoro-2-pyridinyl)-5-methyl-1H-1,2,4-triazol-3-ol. The product melted at 272°-274° C. and upon analysis was found to have carbon, hydrogen and nitrogen contents of 49.58, 3.83 and 28.88 percent, respectively, as compared with the theoretical contents of 49.48, 3.63 and 28.85 percent, respectively, as calculated for the above named compound.

Aufarbeitung

  1. customA solution was prepared
  2. temperatureThe mixture was refluxed overnight
  3. customThe solids which precipitated out
  4. filtrationwere recovered by filtration
  5. washThe solids were washed with methylene chloride
  6. customdried under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-73d1a52c67bf4f41897bcca46de6aa73
Quelldatensatz
uspto-grants-1984_05
Patentnummer
US04451653

Notizen zur Reaktion

Wird geladen…