Sulfuric Acid → HCID 3682022, compound
Reaction equation
ON=[CH:3][C:4]([NH:6][C:7]1[CH:12]=[CH:11][C:10]([O:13][CH3:14])=[CH:9][C:8]=1[N+:15]([O-:17])=[O:16])=[O:5].[OH:18]S(O)(=O)=O>>[CH3:14][O:13][C:10]1[CH:11]=[C:12]2[C:7](=[C:8]([N+:15]([O-:17])=[O:16])[CH:9]=1)[NH:6][C:4](=[O:5])[C:3]2=[O:18]Participants
3
Conditions
- Temperature
- 80 °C
Procedure
2-Hydroxyimino-N-(4-methoxy-2-nitro-phenyl)-acetamide (5 g, 22 mmol) was added portion wise to a hot solution of conc. H2SO4 (20 mL, 4 vol) at 60° C. After completion of the addition, temperature was raised to 80° C. and maintained the same for one hour. After completion of the reaction, the reaction mixture was poured on to the crushed ice and the resulting precipitate separated was filtered, washed with water (2-3 times) and dried under vacuum to obtain the title compound as brick red colored solid which was used directly for the next reaction.
Workup
- additionAfter completion of the addition, temperature
- temperaturemaintained the same for one hour
- customAfter completion of the reaction
- customthe resulting precipitate separated
- filtrationwas filtered
- washwashed with water (2-3 times)
- customdried under vacuum
Sources & evidence
- ORD record
- ord-015494c8b28945968cf754eb8a1f613c
- Source dataset
- uspto-grants-2015_04
- Patent number
- US09006454B2
Reaction notes
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