Methane → HCID 178524636, compound

HRID 469294Notes

Reaction equation

HRID 469294 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 (287 mmol) sodium diethyl-oxalacetate and 30.2 g (287 mmol) formamidine acetate were added to 24.1 g (597 mmol) 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 hot and after cooling acidified with aqueous HCl. The solution was concentrated to dryness by rotary evaporation. The residue contained the desired product and was used in the next step without further purification.

Workup

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

Sources & evidence

ORD record
ord-15bd33570d9b42d79b0b59bd94cdd316
Source dataset
uspto-grants-2014_01
Patent number
US08629137B2

Reaction notes

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