Hydrochloric Acid → HCID 23255692, compound
Reaction equation
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([NH2:9])=[C:5]([N+:10]([O-:12])=[O:11])[CH:4]=1.Cl[C:14](Cl)(Cl)[CH:15]([OH:17])O.S([O-])([O-])(=O)=O.[Na+].[Na+].Cl.[NH2:28][OH:29].Cl>O>[OH:29][N:28]=[CH:14][C:15]([NH:9][C:6]1[CH:7]=[CH:8][C:3]([O:2][CH3:1])=[CH:4][C:5]=1[N+:10]([O-:12])=[O:11])=[O:17]Participants
7
Reactant 5
Product 1
Reagents, catalysts & solvents 1
Procedure
A slurry of 4-methoxy-2-nitro-phenylamine (5 g, 29.7 mmol), chloral hydrate (5.51 g, 33.3 mmol), sodium sulphate (21 g, 148.8 mmol), hydroxylamine hydrochloride (6.6 g, 95.2 mmol) and conc. HCl (5 mL) in water (150 mL) was heated for 2 h. After completion of the reaction, a solid separates out. The reaction mixture was then cooled to room temperature and the solids were filtered, washed with water (2-3 times) and dried under vacuum to obtain the title compound as off white solid (5 g, 70.40%) which was directly used for the next reaction.
Workup
- customAfter completion of the reaction
- filtrationthe solids were filtered
- washwashed with water (2-3 times)
- customdried under vacuum
Sources & evidence
- ORD record
- ord-7670b4aabc3043899db3462631dba141
- Source dataset
- uspto-grants-2015_04
- Patent number
- US09006454B2
Reaction notes
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