Methane → HCID 178524636, compound

HRID 74500Notes

Reaction equation

HRID 74500 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 (0.29 mol) sodium diethyloxalacetate and 30.2 g (0.29 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 hot and after cooling acidified with aqueous hydrochloric acid. The solution was evaporated 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 hot
  3. temperatureafter cooling
  4. customThe solution was evaporated to dryness by rotary evaporation
  5. customwas used in the next step without any further purification

Sources & evidence

ORD record
ord-2e9cf09b7ee849daaace99eaa049e685
Source dataset
uspto-grants-2014_09
Patent number
US08829006B2

Reaction notes

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