Hydroxyamine hydrochloride → HCID 137231663, compound

HRID 2257526Notes

Reaction equation

HRID 2257526 reaction equation
Cl.[NH2:2][OH:3].O.O.O.C([O-])(=O)C.[Na+].[F:12][C:13]1[CH:18]=[C:17]([F:19])[CH:16]=[CH:15][C:14]=1[C:20]([C:22]1[CH:27]=[CH:26][N:25]=[CH:24][CH:23]=1)=O>C(O)C>[F:12][C:13]1[CH:18]=[C:17]([F:19])[CH:16]=[CH:15][C:14]=1[C:20]([C:22]1[CH:27]=[CH:26][N:25]=[CH:24][CH:23]=1)=[N:2][OH:3]

Participants

5

Reactant 3

HCID 443297Hydroxyamine hydrochlorideHCID 22923333HCID 22923333, compoundHCID 23665404Sodium Acetate Trihydrate

Product 1

HCID 137231663HCID 137231663, compoundYield 94.5%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

62.6 g (0.900 mole) of hydroxylamine hydrochloride and 133.6 g (0.982 mole) of sodium acetate trihydrate were added to a suspension of 179.4 g (0.818 mole) of the compound of Example 1 in 1L of ethanol and the mixture was refluxed for 1 hour. The solvent was removed under low pressure evaporation, 1L of water was added to the residue and it was filtered. After drying for 3 hours at 45° C., 181 g (94% yield) of the title compound (mixture of sin- and anti-isomers) were obtained, as a white solid.

Workup

  1. temperaturethe mixture was refluxed for 1 hour
  2. customThe solvent was removed under low pressure evaporation, 1L of water
  3. additionwas added to the residue and it
  4. filtrationwas filtered
  5. customAfter drying for 3 hours at 45° C.

Sources & evidence

ORD record
ord-334910c5c11a4b919cb9fe2d13cf757b
Source dataset
uspto-grants-1997_08
Patent number
US05658916

Reaction notes

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