Acetic Acid → 8-Bromo-1-methyl-[1,2,4]triazolo[4,3-a]quinoxaline
Reaktionsgleichung
[Br:1][C:2]1[CH:11]=[C:10]2[C:5]([N:6]=[CH:7][C:8]([NH:12][NH2:13])=[N:9]2)=[CH:4][CH:3]=1.[C:14](O)(=O)[CH3:15]>>[Br:1][C:2]1[CH:11]=[C:10]2[C:5]([N:6]=[CH:7][C:8]3[N:9]2[C:14]([CH3:15])=[N:13][N:12]=3)=[CH:4][CH:3]=1Komponenten
3
Versuchsvorschrift
A mixture of 7-bromo-2-hydrazinylquinoxaline (1 g, 4.18 mmol) in acetic acid (10 mL) was refluxed for 18 h. Half of the acetic acid was removed under vacuum and the residue was poured into ice-water. The precipitate was collected on a filter, washed with water, and dried under vacuo to afford crude 8-bromo-1-methyl-[1,2,4]triazolo[4,3-a]quinoxaline as a dark red solid (1 g, yield 90%) which was used in the next step without further purification. MS (m/z): 263 (M+H)+.
Aufarbeitung
- temperaturewas refluxed for 18 h
- customHalf of the acetic acid was removed under vacuum
- additionthe residue was poured into ice-water
- customThe precipitate was collected on a filter
- washwashed with water
- customdried under vacuo
Quellen und Nachweise
- ORD-Eintrag
- ord-5d14d82332fb4e68aafe04a1a681c519
- Quelldatensatz
- uspto-grants-2015_11
- Patentnummer
- US09181264B2
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