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Triacetoxyperiodinane → HCID 83598147、化合物

HRID 1877106
ノート
印刷プレビュー

反応式

HRID 1877106 の反応式
CC(OI1(OC(C)=O)(OC(C)=O)[O:14][C:12](=O)[C:11]2[CH:10]=[CH:9][CH:8]=[CH:7][C:6]1=2)=O>O>[CH2:7]([C:6]1[O:14][C:12]([C:11]2[CH:6]=[CH:7][CH:8]=[CH:9][CH:10]=2)=[CH:10][C:11]=1[CH:12]=[O:14])[CH3:8]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

3

反応物 1

HCID 159087Triacetoxyperiodinane

生成物 1

HCID 83598147HCID 83598147、化合物収率 137.4%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
0 °C

実験手順

To a solution of (2-ethyl-5-phenylfuran-3-yl)methanol (5.9 g) obtained by the above-mentioned reaction in methylene chloride (30 mL) was added Dess-Martin reagent (14.8 g) at 0° C., and the mixture was stirred at 0° C. for 2 hr. The reaction mixture was poured into water, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated aqueous sodium hydrogen carbonate, and dried over magnesium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel chromatography (0% ethyl acetate/hexane to 25% ethyl acetate/hexane) to give the title compound (4.8 g, 83%) as an oil.

後処理

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe organic layer was washed with saturated aqueous sodium hydrogen carbonate
  3. dry with materialdried over magnesium sulfate
  4. customThe solvent was evaporated under reduced pressure
  5. customthe residue was purified by silica gel chromatography (0% ethyl acetate/hexane to 25% ethyl acetate/hexane)

出典と根拠

ORDレコード
ord-be8812ff66404788b49dc71de034a884
出典データセット
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08309580B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート