Ethyl orthoformate → HCID 13385702, Verbindung
Reaktionsgleichung
[Cl:1][C:2]1[C:11]([NH:12][NH2:13])=[N:10][C:9]2[C:4](=[CH:5][C:6]([F:15])=[C:7]([F:14])[CH:8]=2)[N:3]=1.[CH:16](OCC)(OCC)OCC>>[Cl:1][C:2]1[C:11]2[N:10]([CH:16]=[N:13][N:12]=2)[C:9]2[C:4]([N:3]=1)=[CH:5][C:6]([F:15])=[C:7]([F:14])[CH:8]=2Komponenten
3
Versuchsvorschrift
A mixture consisting of 5.99 g. (0.026 mole) of 2-chloro-6,7-difluoro-3-hydrazinoquinoxaline and 30 ml. (0.18 mole) of triethyl orthoformate was heated at 100° C. for a period of 24 hours to give a red-brown solid. The resulting slurry was then cooled to room temperature and filtered, and the recovered product subsequently washed with diethyl ether to ultimately afford 5.15 g. (82%) of pure 4-chloro-7,8-difluoro-[1,2,4]triazolo[4,3-a]quinoxaline, m.p. >210° C. (decomp.). Mass Spectrum: m/e, 242/240 (P+).
Aufarbeitung
- customto give a red-brown solid
- filtrationfiltered
- washthe recovered product subsequently washed with diethyl ether to ultimately afford 5.15 g