Triethyl orthoacetate → 4,8-Dichloro-1-methyl-[1,2,4]triazolo[4,3-a]quinoxaline

HRID 464277Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 464277
[Cl:1][C:2]1[C:11]([NH:12][NH2:13])=[N:10][C:9]2[C:4](=[CH:5][CH:6]=[C:7]([Cl:14])[CH:8]=2)[N:3]=1.[C:15](OCC)(OCC)(OCC)[CH3:16]>>[Cl:1][C:2]1[C:11]2[N:10]([C:15]([CH3:16])=[N:13][N:12]=2)[C:9]2[C:4]([N:3]=1)=[CH:5][CH:6]=[C:7]([Cl:14])[CH:8]=2

Komponenten

3

Edukt 2

HCID 66221Triethyl orthoacetateHCID 14733462,6-Dichloro-3-hydrazinylquinoxaline

Produkt 1

HCID 133857034,8-Dichloro-1-methyl-[1,2,4]triazolo[4,3-a]quinoxaline

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

A mixture consisting of 20 g. (0.087 mole) of 2,6-dichloro-3-hydrazinoquinoxaline and 160 ml. (0.87 mole) of triethyl orthoacetate was heated with mechanical stirring under a dry nitrogen atmosphere in a preheated oil bath at 100° C. for a period of 20 hours to give a yellow suspension. The resulting mixture was cooled to room temperature and filtered, and the recovered solid product was subsequently washed with ethanol and air-dried to constant weight to ultimately afford 10.2 g. (46%) of pure 4,8-dichloro-1-methyl-[1,2,4]triazolo[4,3-a]quinoxaline, m.p. >280° C. Mass Spectrum: m/e, 254/252 (P+).

Aufarbeitung

  1. customto give a yellow suspension
  2. temperatureThe resulting mixture was cooled to room temperature
  3. filtrationfiltered
  4. washthe recovered solid product was subsequently washed with ethanol
  5. customair-dried to constant weight to ultimately afford 10.2 g

Quellen und Nachweise

ORD-Eintrag
ord-85bb29ef69c2481983279590ea59f397
Quelldatensatz
uspto-grants-1985_10
Patentnummer
US04547501

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