Methane → HCID 21548009, compound

HRID 1604875Notes

Reaction equation

HRID 1604875 reaction equation
[NH2:1][C:2]1[CH:3]=[N:4][C:5]([C:9](=[O:11])N)=[C:6]([NH2:8])[N:7]=1.C.[OH-:13].[Na+]>O>[NH2:8][C:6]1[C:5]([C:9]([OH:11])=[O:13])=[N:4][CH:3]=[C:2]([NH2:1])[N:7]=1

Participants

5

Reactant 3

HCID 297MethaneHCID 14798Sodium HydroxideHCID 21548006HCID 21548006, compound

Product 1

HCID 21548009HCID 21548009, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

A slurry consisting of 1.60 g of 3,5-diamino-6-carbamoylpyrazine, from Example 4, in 20 ml of 10% aqueous sodium hydroxide was heated at reflux for 2 hours, diluted to 100 ml with hot water and the resulting homogeneous solution was decolorized with Darco. Careful acidification to pH 1 gave a precipitate which was collected from the chilled solution by filtration. The collected material was washed twice, each time with small portions of water and methanol and dried yielding 0.92 g of 3,5-diaminopyrazinoic acid as a light powder, mp 169° (dec.).

Workup

  1. temperaturewas heated
  2. temperatureat reflux for 2 hours
  3. customCareful acidification to pH 1 gave a precipitate which
  4. filtrationwas collected from the chilled solution by filtration
  5. washThe collected material was washed twice
  6. dry with materialeach time with small portions of water and methanol and dried

Sources & evidence

ORD record
ord-9d29c0cbe2644a8b8d029a818ac7130c
Source dataset
uspto-grants-1976_04
Patent number
US03948895

Reaction notes

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