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Ethanol → 4-Ethyl-2,4-hexadien-1-ylamine

HRID 2295002
Notes
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Reaction equation

HRID 2295002 reaction equation
[CH2:1]([C:3](=[CH:18][CH3:19])[CH:4]=[CH:5][CH2:6][N:7]1C(=O)C2=CC=CC=C2C1=O)[CH3:2].O.NN.C(O)C>[OH-].[Na+]>[CH2:18]([C:3](=[CH:1][CH3:2])[CH:4]=[CH:5][CH2:6][NH2:7])[CH3:19]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 3

HCID 702EthanolHCID 24654Hydrazine hydrate (1:1)HCID 54389132N-(4-ethyl-2,4-hexadien-1-yl)phthalimide

Product 1

HCID 539452134-Ethyl-2,4-hexadien-1-ylamine

Reagents, catalysts & solvents 1

HCID 14798Sodium HydroxideSolvent

Procedure

A mixture of N-(4-ethyl-2,4-hexadien-1-yl)phthalimide (3.0 g), hydrazine monohydrate (0.88 g), and ethanol (30 ml) was refluxed for 40 minutes under nitrogen atmosphere. After cooling, the precipitate was filtered and washed with ethanol. Evaporation of the filtrate gave a crystalline residue which was dissolved in 1N sodium hydroxide solution and extracted with dichloromethane. The organic extract was washed with water and brine, dried over anhydrous sodium sulfate, and evaporated to give 4-ethyl-2,4-hexadien-1-ylamine as an oil. To a mixture of crude 4-ethyl-2,4-hexadien-1-ylamine, triethylamine 1.79 g), and dichloromethane (30 ml) at 0° C. was added dropwise dimethylsulfamoyl chloride (2.03 g) during 10 minutes. After 30 minutes, triethylamine (0.6 g) and dimethylsulfamoyl chloride (0.85 g) were added to the reaction mixture. After 1 hour at 0° C., the reaction mixture was washed with water and aqueous sodium hydrogen carbonate solution, dried over anhydrous magnesium sulfate, and evaporated in vacuo. The residue was chromatographed on silica gel (dichloromethane-hexane, 7:3) to give N,N-dimethyl-N'-(4-ethyl-2,4-hexadien-1-yl)-sulfamide (924 mg) as an oil.

Workup

  1. temperaturewas refluxed for 40 minutes under nitrogen atmosphere
  2. temperatureAfter cooling
  3. filtrationthe precipitate was filtered
  4. washwashed with ethanol
  5. customEvaporation of the filtrate
  6. customgave a crystalline residue which
  7. extractionextracted with dichloromethane
  8. extractionThe organic extract
  9. washwas washed with water and brine
  10. dry with materialdried over anhydrous sodium sulfate
  11. customevaporated

Sources & evidence

ORD record
ord-30111c38b5ba4252952d195f5b78de66
Source dataset
uspto-grants-1997_11
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US05691366

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes