Hydrochloric Acid → HCID 23255692, compound

HRID 1470585Notes

Reaction equation

HRID 1470585 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

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

  1. customAfter completion of the reaction
  2. filtrationthe solids were filtered
  3. washwashed with water (2-3 times)
  4. customdried under vacuum

Sources & evidence

ORD record
ord-7670b4aabc3043899db3462631dba141
Source dataset
uspto-grants-2015_04
Patent number
US09006454B2

Reaction notes

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