Hydrazine hydrate (1:1) → HCID 178470317, compound

HRID 352823Notes

Reaction equation

HRID 352823 reaction equation
[C:1]([O:6][CH2:7][CH3:8])(=S)[C:2]([NH2:4])=O.[OH2:9].[NH2:10][NH2:11].O.[N:13]1[CH:18]=[CH:17][C:16]([C:19](=O)[C:20]([O:22]CC)=O)=[CH:15][CH:14]=1>C(O)C>[O:22]=[C:20]1[C:19]([C:16]2[CH:17]=[CH:18][N:13]=[CH:14][CH:15]=2)=[N:11][NH:10][C:2]([C:1]([O:6][CH2:7][CH3:8])=[O:9])=[N:4]1

Participants

5

Reactant 3

HCID 24654Hydrazine hydrate (1:1)HCID 216137632-ethoxy-2-thioxoAcetamideHCID 86592084Ethyl (pyridin-4-yl)glyoxylate Hydrate

Product 1

HCID 178470317HCID 178470317, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

Ethyl thiooxamate (172 mg) was suspended in ethanol (5 ml) at 0° C., followed by the addition of hydrazine monohydrate (63 μl). While the resulting gas was suctioned, the resulting mixture was stirred for 30 minutes. Ethyl (pyridin-4-yl)glyoxylate hydrate (254 mg) was added to the reaction mixture and the mixture was stirred at room temperature for 30 minutes. After heating under reflux for 4 hours, the reaction mixture was concentrated. The yellow powder thus precipitated was collected by filtration and dried, whereby the title compound (140 mg) was obtained.

Workup

  1. stirringthe mixture was stirred at room temperature for 30 minutes
  2. temperatureAfter heating
  3. temperatureunder reflux for 4 hours
  4. concentrationthe reaction mixture was concentrated
  5. customThe yellow powder thus precipitated
  6. filtrationwas collected by filtration
  7. customdried

Sources & evidence

ORD record
ord-cc172d11b08d4c619986306802748eac
Source dataset
uspto-grants-2004_06
Patent number
US06747023B1

Reaction notes

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