Hydroxyamine hydrochloride → HCID 73183059, compound

HRID 903896Notes

Reaction equation

HRID 903896 reaction equation
[CH2:1]=[C:2]1[C:8]2[CH:9]=[N:10][CH:11]=[CH:12][C:7]=2[CH2:6][C:5](=O)[C:4]2[CH:14]=[CH:15][CH:16]=[CH:17][C:3]1=2.C([O-])(=O)C.[Na+].Cl.[NH2:24][OH:25]>CO>[CH2:1]=[C:2]1[C:8]2[CH:9]=[N:10][CH:11]=[CH:12][C:7]=2[CH2:6][C:5](=[N:24][OH:25])[C:4]2[CH:14]=[CH:15][CH:16]=[CH:17][C:3]1=2

Participants

5

Reactant 3

HCID 443297Hydroxyamine hydrochlorideHCID 517045Sodium AcetateHCID 13464030HCID 13464030, compound

Product 1

HCID 73183059HCID 73183059, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

A mixture of the ketone from Step E (6.2 g.), anhydrous sodium acetate (3.1 g.), hydroxylamine hydrochloride (2.48 g.) and CH3OH (130 ml.) is heated under reflux for 24 hours. The solvent is removed in vacuo, water (100 ml.) is added to the residue and the resulting yellow-orange solid is collected and dried, 6.4 g., m.p. 183°-205° C. Recrystallization from toluene provides material with m.p. 218.5°-221° C. (dec.).

Workup

  1. temperatureis heated
  2. temperatureunder reflux for 24 hours
  3. customThe solvent is removed in vacuo, water (100 ml.)
  4. additionis added to the residue
  5. customthe resulting yellow-orange solid is collected
  6. customdried
  7. customRecrystallization from toluene
  8. customprovides material with m.p. 218.5°-221° C. (dec.)

Sources & evidence

ORD record
ord-82854b8117164538ad16185580e369d8
Source dataset
uspto-grants-1980_10
Patent number
US04229455

Reaction notes

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