Azane;hydrate → [1,2,4]Triazolo[4,3-a]quinazoline, 1-methyl-7-nitro-5-phenyl-
Reaction equation
[C:1]([NH:4][NH:5][C:6]1[N:15]=[C:14]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[C:13]2[C:8](=[CH:9][CH:10]=[C:11]([N+:22]([O-:24])=[O:23])[CH:12]=2)[N:7]=1)(=O)[CH3:2].O.N>>[CH3:2][C:1]1[N:7]2[C:8]3[C:13]([C:14]([C:16]4[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=4)=[N:15][C:6]2=[N:5][N:4]=1)=[CH:12][C:11]([N+:22]([O-:24])=[O:23])=[CH:10][CH:9]=3Participants
3
Procedure
In the next place, a mixture of 0.8 g of 2-(2-acetylhydrazino)-4-phenyl-6-nitroquinazoline thus obtained and 16 g of polyphosphoric acid was heated at 150° to 160° C for 2 hours. The mixture was then poured into ice-water and made alkaline with concentrated ammonia water. The precipitated crystals were filtered, washed with ethanol and then recrystallized from chloroform to obtain 1-methyl-5-phenyl-7-nitro-s-triazolo[4,3-a]quinazoline as pale brown crystals, m.p. 350° - 352° C.
Workup
- customthus obtained
- filtrationThe precipitated crystals were filtered
- washwashed with ethanol
- customrecrystallized from chloroform
Sources & evidence
- ORD record
- ord-497f79310f29445da908c0d1bf87134e
- Source dataset
- uspto-grants-1977_01
- Patent number
- US04002755
Reaction notes
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