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

HRID 31676
ノート
印刷プレビュー

反応式

HRID 31676 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

HCID 597925263-Ethyl-2-methylpyridine1-oxide収率 89.6%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-8aabbf1aa12a4bc8be4bfd05ef2cb690
出典データセット
uspto-grants-2008_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07425634B2

反応ノート

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