O-Methylhydroxylamine hydrochloride → HCID 54097963, compound

HRID 2286666Notes

Reaction equation

HRID 2286666 reaction equation
Cl.[CH3:2][O:3][NH2:4].[NH2:5][C:6]1[CH:11]=[CH:10][N:9]=[C:8]([C:12](=O)[C:13]([O-:15])=[O:14])[N:7]=1.[K+]>CO>[NH2:5][C:6]1[CH:11]=[CH:10][N:9]=[C:8]([C:12](=[N:4][O:3][CH3:2])[C:13]([OH:15])=[O:14])[N:7]=1

Participants

4

Reactant 2

HCID 521874O-Methylhydroxylamine hydrochlorideHCID 23690652HCID 23690652, compound

Product 1

HCID 54097963HCID 54097963, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

To a solution of O-methylhydroxylamine hydrochloride (0.25 g.) in methanol (6 ml.) was added a mixture of potassium 2-(4-aminopyrimidin-2-yl)glyoxylate and its monohydrate with stirring at ambient temperature, and the mixture was stirred for 4 hours. The reaction mixture was allowed to stand overnight at ambient temperature, filtered, and the filtered precipitates were washed with ethanol. After the filtrate and washings were combined together, the solvents were distilled off. The resultant oily substance was pulverized in acetone (15 ml.) and collected by filtration. Thus obtained powder was washed successively with acetone and diethyl ether and then dried to give a pale brown powder of 2-(4-aminopyrimidin-2-yl)-2-methoxyiminoacetic acid (syn isomer) (290 mg.).

Workup

  1. stirringthe mixture was stirred for 4 hours
  2. filtrationfiltered
  3. customthe filtered precipitates
  4. washwere washed with ethanol
  5. distillationthe solvents were distilled off
  6. filtrationcollected by filtration
  7. washThus obtained powder was washed successively with acetone and diethyl ether
  8. customdried

Sources & evidence

ORD record
ord-2949233f16814649b6eb19cd5f692a4a
Source dataset
uspto-grants-1981_05
Patent number
US04267176

Reaction notes

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