Hydrazine hydrate (1:1) → HCID 15289680, compound

HRID 37502Notes

Reaction equation

HRID 37502 reaction equation
[NH2:1][C:2]1[C:3]([C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)=[N:4][C:5]([N:18]2[CH:22]=[N:21][CH:20]=[N:19]2)=[C:6]([C:13](OCC)=[O:14])[C:7]=1[C:8]([O:10]CC)=O.O.[NH2:30][NH2:31]>C(O)C>[NH2:1][C:2]1[C:7]2[C:8](=[O:10])[NH:31][NH:30][C:13](=[O:14])[C:6]=2[C:5]([N:18]2[CH:22]=[N:21][CH:20]=[N:19]2)=[N:4][C:3]=1[C:23]1[CH:24]=[CH:25][CH:26]=[CH:27][CH:28]=1

Participants

4

Reactant 2

HCID 24654Hydrazine hydrate (1:1)HCID 152897013-Amino-4,5-diethoxycarbonyl-2-phenyl-6-(1,2,4-triazol-1-yl)pyridine

Product 1

HCID 15289680HCID 15289680, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

In 15 ml of ethanol was dissolved 0.215 g of 3-amino-4,5-diethoxycarbonyl-2-phenyl-6-(1,2,4-triazol-1-yl)pyridine, whereto 1 ml of hydrazine monohydrate was added. The mixture was heated under reflux for 7 hours. After cooling, the resulting yellow crystals were collected by filtration and washed with ethanol. The crystals were suspended in 20 ml of water and the suspension was acidified by addition of 1 ml of acetic acid. Thereafter, the crystals were collected by filtration, washed with water and dried to give 0.11 g of the title compound.

Workup

  1. additionwas added
  2. temperatureThe mixture was heated
  3. temperatureunder reflux for 7 hours
  4. temperatureAfter cooling
  5. filtrationthe resulting yellow crystals were collected by filtration
  6. washwashed with ethanol
  7. additionthe suspension was acidified by addition of 1 ml of acetic acid
  8. filtrationThereafter, the crystals were collected by filtration
  9. washwashed with water
  10. customdried

Sources & evidence

ORD record
ord-a3abfe37ed4d441993b5516fb8684599
Source dataset
uspto-grants-1995_05
Patent number
US05420275

Reaction notes

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