Ethanol → HCID 178469369, compound

HRID 743679Notes

Reaction equation

HRID 743679 reaction equation
S(=O)(=O)(O)O.[CH3:6][NH:7][NH2:8].C([C:11](CC)([C:15]([C:17]([O-:19])=[O:18])=O)[C:12]([O-:14])=O)C.[Na+].[Na+].[CH2:24](O)[CH3:25]>>[CH2:24]([O:19][C:17]([C:15]1[CH:11]=[C:12]([OH:14])[N:7]([CH3:6])[N:8]=1)=[O:18])[CH3:25]

Participants

5

Reactant 4

HCID 702EthanolHCID 1118Sulfuric AcidHCID 6061MethylhydrazineHCID 23179480Diethyloxalacetate sodium

Product 1

HCID 178469369HCID 178469369, compound

Procedure

To 800 ml of ethanol were added 108 g (1.1 mol) of sulfuric acid, 92.1 g (2.0 mol) of methylhydrazine, and 462.4 g (2.20 mol) of sodium diethyloxalacetate. This mixture was stirred at room temperature for 2 hours, and then heated with refluxing and stirring for 3 hours. After the ethanol was distilled off, 800 ml of water was added to the residue. The resulting mixture was allowed to stand at room temperature overnight, and the crystals yielded were taken out by filtration and washed with water. Yield: 279 g (82%). Melting point: 151°-153° C.

Workup

  1. temperatureheated
  2. temperaturewith refluxing
  3. stirringstirring for 3 hours
  4. distillationAfter the ethanol was distilled off
  5. addition800 ml of water was added to the residue
  6. waitto stand at room temperature overnight
  7. customthe crystals yielded
  8. filtrationwere taken out by filtration
  9. washwashed with water

Sources & evidence

ORD record
ord-e1820d41407d48b2975d49ba2fe9921f
Source dataset
uspto-grants-1996_09
Patent number
US05556987

Reaction notes

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