Methane → HCID 178524636, compound

HRID 1640229Notes

Reaction equation

HRID 1640229 reaction equation
C([C:3](CC)([C:7]([C:9]([O-:11])=[O:10])=O)[C:4]([O-])=[O:5])C.[Na+].[Na+].C(O)(=O)C.[CH:20]([NH2:22])=[NH:21].[OH-].[Na+].C>O>[OH:5][C:4]1[N:22]=[CH:20][N:21]=[C:7]([C:9]([OH:11])=[O:10])[CH:3]=1

Participants

6

Reactant 4

HCID 297MethaneHCID 14798Sodium HydroxideHCID 160693Formamidine acetateHCID 23179480Diethyloxalacetate sodium

Product 1

HCID 178524636HCID 178524636, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

63.5 g (0.3 mol) sodium diethyloxalacetate and 30.2 g (0.3 mol) formamidine acetate were added to 24.1 g (0.6 mol) NaOH in 3.6 L water. The mixture was stirred overnight at RT. Then activated charcoal was added and the mixture was refluxed for 1 h. It was filtered off while hot and after cooling acidified with a hydrochloric acid solution. The solution was concentrated to dryness by rotary evaporation. The residue contained the desired product and was used in the next step without any further purification.

Workup

  1. temperaturethe mixture was refluxed for 1 h
  2. filtrationIt was filtered off while hot and
  3. temperatureafter cooling
  4. concentrationThe solution was concentrated to dryness by rotary evaporation
  5. customwas used in the next step without any further purification

Sources & evidence

ORD record
ord-e2477d4606244d10b782926dfe94510e
Source dataset
uspto-grants-2012_02
Patent number
US08110575B2

Reaction notes

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