O-Methylhydroxylamine hydrochloride → HCID 54097963, compound

HRID 1982698Notes

Reaction equation

HRID 1982698 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. This 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. washThis obtained powder was washed successively with acetone and diethyl ether
  8. customdried

Sources & evidence

ORD record
ord-df572eb643024f6e9c29f24bf3d42b66
Source dataset
uspto-grants-1986_06
Patent number
US04596869

Reaction notes

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