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Butanal → N-Butyl-2-pyridinamine

HRID 1881032
Notes
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Reaction equation

HRID 1881032 reaction equation
[NH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][N:3]=1.[CH:8](=O)[CH2:9][CH2:10][CH3:11].C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].C(OCC)(=O)C>C(Cl)(Cl)Cl.C(O)(=O)C>[CH2:8]([NH:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][N:3]=1)[CH2:9][CH2:10][CH3:11]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

7

Reactant 4

HCID 261ButanalHCID 8857Ethyl AcetateHCID 104392-AminopyridineHCID 5049666Sodium triacetoxyborohydride

Product 1

HCID 14322668N-Butyl-2-pyridinamineYield 34%

Reagents, catalysts & solvents 2

HCID 176Acetic Acid
Solvent
HCID 6212ChloroformSolvent

Procedure

2-aminopyridine (5.0 g) was dissolved in chloroform (40 mL) and acetic acid (10 mL), and n-butyraldehyde (4.2 g) was added, then stirred at room temperature for 30 minutes. Sodium triacetoxyborohydride (16.9 g) was added and stirred at room temperature for three hours. Ethyl acetate (300 mL) was added to the reaction solution, and the organic layer was washed with saturated aqueous solution of sodium hydrogen carbonate (200 mL) and saturated sodium chloride solution (50 mL). After drying on anhydrous sodium sulfate, filtration, and vacuum concentration, the residue was purified by silica gel flash column chromatography (developing solvent: n-hexane:ethyl acetate=2:1) to give the above-identified compound (2.7 g, yield 34%).

Workup

  1. stirringstirred at room temperature for three hours
  2. washthe organic layer was washed with saturated aqueous solution of sodium hydrogen carbonate (200 mL) and saturated sodium chloride solution (50 mL)
  3. dry with materialAfter drying on anhydrous sodium sulfate, filtration, and vacuum concentration
  4. customthe residue was purified by silica gel flash column chromatography (developing solvent: n-hexane:ethyl acetate=2:1)

Sources & evidence

ORD record
ord-bd12a45927eb449fa724f4756949b782
Source dataset
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US08318781B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes