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

HRID 31676
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HRID 31676 반응식
[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]
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참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-8aabbf1aa12a4bc8be4bfd05ef2cb690
출처 데이터셋
uspto-grants-2008_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07425634B2

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