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3-Ethyl-2-methylpyridine → 3-Ethyl-2-methylpyridine1-oxide

HRID 31676
Notes
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Reaction equation

HRID 31676 reaction equation
[CH2:1]([C:3]1[C:4]([CH3:9])=[N:5][CH:6]=[CH:7][CH:8]=1)[CH3:2].ClC1C=CC=C(C(OO)=[O:18])C=1.C(=O)([O-])O.[Na+]>ClCCl>[CH2:1]([C:3]1[C:4]([CH3:9])=[N+:5]([O-:18])[CH:6]=[CH:7][CH:8]=1)[CH3:2]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 3

HCID 340873-Ethyl-2-methylpyridineHCID 70297m-Chloroperbenzoic acidHCID 516892Sodium Bicarbonate

Product 1

HCID 597925263-Ethyl-2-methylpyridine1-oxideYield 89.6%

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

First, 3-ethyl-2-methylpyridine (7.25 g, 59.8 mmol) was dissolved in dichloromethane (dehydrated)(100 ml) and 3-chloroperbenzoic acid (19.0 g, 71.6 mmol, as the content was regarded as 65%) was added in a nitrogen atmosphere at ice-cooling temperature. The mixture was stirred at room temperature for 90 hours. To the reaction mixture, a saturated aqueous sodium hydrogen carbonate solution was added. The aqueous layer was extracted twice with dichloromethane and three times with chloroform. The organic layers were combined, dried over anhydrous magnesium sulfate, filtrated and concentrated. The residue was purified by silica gel column chromatography (silica gel: 100 g, elution solvent: heptane, ethyl acetate/methanol=10/1) to obtain the title compound (7.35 g, yield: 89.6%) as a reddish solid.

Workup

  1. additionwas added in a nitrogen atmosphere at ice-
  2. temperaturecooling temperature
  3. extractionThe aqueous layer was extracted twice with dichloromethane and three times with chloroform
  4. dry with materialdried over anhydrous magnesium sulfate
  5. filtrationfiltrated
  6. concentrationconcentrated
  7. customThe residue was purified by silica gel column chromatography (silica gel: 100 g, elution solvent: heptane, ethyl acetate/methanol=10/1)

Sources & evidence

ORD record
ord-8aabbf1aa12a4bc8be4bfd05ef2cb690
Source dataset
uspto-grants-2008_09
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US07425634B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes