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

HRID 2295001
Notes
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Reaction equation

HRID 2295001 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-ylamineYield 105.6%

Reagents, catalysts & solvents 1

HCID 14798Sodium HydroxideSolvent

Procedure

A mixture of N-(4-ethyl-2,4-hexadien-1-yl)phthalimide (5.0 g), hydrazine monohydrate (2.45 g), and ethanol (150 ml) was refluxed for 1.5 hours 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 crude 4-ethyl-2,4-hexadien-1-ylamine (2.59 g) as an oil. The crude oil was dissolved in dichloromethane (30 ml) containing triethylamine (6.28 g). To this solution cooled to 0° C. was added nicotinic acid chloride hydrochloride (3.41 g) in small portions during 10 minutes. After 30 minutes, triethylamine (4.19 g) and nicotinic acid chloride hydrochloride (0.79 g) were added and the mixture was stirred for 30 minutes at 0° C. The reaction mixture was diluted with dichloromethane, washed with water and brine, dried over anhydrous magnesium sulfate, and evaporated in vacuo. The residue was chromatographed on silica gel (2% methanol-dichloro-methane) to give a mixture of N-[(2E,4E) and (2Z,4E)-4-ethyl-2,4-hexadien-1-yl]-3-pyridinecarboxamide (4.6 g) which crystallized on standing.

Workup

  1. temperaturewas refluxed for 1.5 hours 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-e95b0fc1d0d14f6998f942307887aadb
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