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Formaldehyde → 1-(1-Ethyl-1H-pyrrol-2-yl)-N,N-dimethylmethanamine

HRID 1269416
Notes
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Reaction equation

HRID 1269416 reaction equation
[CH2:1]=O.Cl.[CH3:4][NH:5][CH3:6].[CH2:7]([N:9]1[CH:13]=[CH:12][CH:11]=[CH:10]1)[CH3:8]>[OH-].[Na+]>[CH3:4][N:5]([CH2:1][C:10]1[N:9]([CH2:7][CH3:8])[CH:13]=[CH:12][CH:11]=1)[CH3:6]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 3

HCID 712FormaldehydeHCID 10473Dimethylamine, hydrochlorideHCID 1852261-Ethylpyrrole

Product 1

HCID 450883351-(1-Ethyl-1H-pyrrol-2-yl)-N,N-dimethylmethanamineYield 97.6%

Reagents, catalysts & solvents 1

HCID 14798Sodium HydroxideSolvent

Procedure

A mixture of 35% aqueous formaldehyde solution (9 ml, 105 mmol) and dimethylamine hydrochloride (9.0 g, 110 mmol) was added to 1-ethylpyrrole (10.0 g, 105 mmol) with stirring under ice-cooling over a 90-minute interval, and then the resulting mixture was stirred at room temperature for 6 hours. After stirring, 10% aqueous sodium hydroxide solution (150 ml) was added to the reaction mixture, and the resulting mixture was extracted with ether. The extract was washed with saturated aqueous sodium chloride solution and dried over anhydrous sodium sulfate. After filtration, the solvent was removed in vacuo, and the residue was purified by chromatography on a silica gel column using a mixed solvent of dichloromethane and methanol (9:1) as the eluent to afford 2-(N,N-dimethylaminomethyl)-1-ethylpyrrole (15.6 g, yield: 97%).

Workup

  1. temperaturecooling over a 90-minute interval
  2. stirringthe resulting mixture was stirred at room temperature for 6 hours
  3. stirringAfter stirring
  4. extractionthe resulting mixture was extracted with ether
  5. washThe extract was washed with saturated aqueous sodium chloride solution
  6. dry with materialdried over anhydrous sodium sulfate
  7. filtrationAfter filtration
  8. customthe solvent was removed in vacuo
  9. customthe residue was purified by chromatography on a silica gel column

Sources & evidence

ORD record
ord-f4871769685f46cbbd45fa8df4700730
Source dataset
uspto-grants-2007_04
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US07199150B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes