Hydrochloric Acid → HCID 6400930, compound

HRID 1470590Notes

Reaction equation

HRID 1470590 reaction equation
[F:1][C:2]1[CH:7]=[CH:6][C:5]([NH2:8])=[CH:4][CH:3]=1.Cl[C:10](Cl)(Cl)[CH:11]([OH:13])O.S([O-])([O-])(=O)=O.[Na+].[Na+].Cl.[NH2:24][OH:25].Cl>O>[F:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:11](=[O:13])[CH:10]=[N:24][OH:25])=[CH:4][CH:3]=1

Participants

7

Reactant 5

HCID 313Hydrochloric AcidHCID 2707Chloral HydrateHCID 97314-FluoroanilineHCID 24436Sodium SulfateHCID 443297Hydroxyamine hydrochloride

Product 1

HCID 6400930HCID 6400930, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Conditions

Temperature
85 °C

Procedure

To a slurry of 4-fluoro-phenylamine (5 g, 45.0 mmol) in water (150 mL), was added chloral hydrate (11.28 g, 67.56 mmol), sodium sulphate (31.97 g, 225.2 mmol), hydroxylamine hydrochloride (6.21, 90.0 mmol), conc. HCl (5 mL) and the reaction mixture was heated to 85° C. It was stirred for another 2 h at the same temperature. After completion of the reaction, a solid separated out. The reaction mixture was cooled to room temperature and filtered, washed with water (2-3 times) and dried to obtain the title compound as off white solid.

Workup

  1. customAfter completion of the reaction
  2. customa solid separated out
  3. temperatureThe reaction mixture was cooled to room temperature
  4. filtrationfiltered
  5. washwashed with water (2-3 times)
  6. customdried

Sources & evidence

ORD record
ord-95b517d534c84a53a9c66670ef4401b3
Source dataset
uspto-grants-2015_04
Patent number
US09006454B2

Reaction notes

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