Methane → HCID 178524636, compound

HRID 2096357Notes

Reaction equation

HRID 2096357 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 (0.597 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 while 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 any further purification.

Workup

  1. temperaturethe mixture was refluxed for 1 h
  2. filtrationIt was filtered 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-236a86f6ecac4252aa756b78363fbe3a
Source dataset
uspto-grants-2013_05
Patent number
US08450327B2

Reaction notes

Loading…