Hydrazine, dihydrochloride → HCID 15480333, compound

HRID 1741255Notes

Reaction equation

HRID 1741255 reaction equation
[CH2:1]([CH:3]([C:11](=O)[C:12]1[C:17]([CH3:18])=[CH:16][C:15]([CH3:19])=[CH:14][C:13]=1[CH3:20])[C:4](=O)[C:5]([O:7][CH2:8][CH3:9])=[O:6])[CH3:2].Cl.Cl.[NH2:24][NH2:25]>CCO>[CH2:1]([C:3]1[C:11]([C:12]2[C:17]([CH3:18])=[CH:16][C:15]([CH3:19])=[CH:14][C:13]=2[CH3:20])=[N:24][NH:25][C:4]=1[C:5]([O:7][CH2:8][CH3:9])=[O:6])[CH3:2]

Participants

4

Reactant 2

HCID 17548Hydrazine, dihydrochlorideHCID 15870414HCID 15870414, compound

Product 1

HCID 15480333HCID 15480333, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Conditions

Temperature
80 °C

Procedure

A mixture of ethyl 3-ethyl-2,4-dioxo-4-(2,4,6trimethylphenyl)butanoate (6.0 g, 20.7 mmol) and hydrazine dihydrochloride (2.17 g, 20.7 mmoL) in 100 mL of EtOH was stirred at 80° C. for 6 hours. The solvent was then removed from the mixture. 200 mL of water was added to the residue and mixture was neutralized by the addition of solid NaHCO3. The product was extracted into ether. The ether extract was dried over Na2SO4 and evaporated to give 5.8 g as an oil which was used in the next reaction without farther purification.

Workup

  1. customThe solvent was then removed from the mixture
  2. addition200 mL of water was added to the residue and mixture
  3. additionwas neutralized by the addition of solid NaHCO3
  4. extractionThe product was extracted into ether
  5. extractionThe ether extract
  6. dry with materialwas dried over Na2SO4
  7. customevaporated
  8. customto give 5.8 g as an oil which
  9. customwas used in the next reaction without farther purification

Sources & evidence

ORD record
ord-5616ef379a354c0facc65c10679039f9
Source dataset
uspto-grants-1999_10
Patent number
US05973152

Reaction notes

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