Hydrazine, dihydrochloride → HCID 15480333, compound

HRID 365487Notes

Reaction equation

HRID 365487 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-(2,4,6-trimethylphenyl)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 further 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 further purification

Sources & evidence

ORD record
ord-0fa899dab5244aa5a9449ba314c26d58
Source dataset
uspto-grants-2000_10
Patent number
US06127399

Reaction notes

Loading…