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Diethyl Carbonate → HCID 89586101、化合物

HRID 1747787
ノート
印刷プレビュー

反応式

HRID 1747787 の反応式
[C:1](=[O:8])([O:5][CH2:6][CH3:7])OCC.[H-].[Na+].[C:11]1([N:17]2[C:21]([C:22](=[O:24])[CH3:23])=[CH:20][CH:19]=[N:18]2)[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1>O>[O:24]=[C:22]([C:21]1[N:17]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[N:18]=[CH:19][CH:20]=1)[CH2:23][C:1]([O:5][CH2:6][CH3:7])=[O:8]
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 7766Diethyl CarbonateHCID 24758Sodium hydrideHCID 534219791-(1-Phenyl-1H-pyrazol-5-yl)ethan-1-one

生成物 1

HCID 89586101HCID 89586101、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a mixture of diethyl carbonate (20.0 mL) and 60% NaH (0.34 g) was added 1-(1-phenyl-1H-pyrazol-5-yl)ethanone (1.30 g) at room temperature, and the mixture was heated under reflux for 2 hr. To the reaction mixture was added water, and the mixture was extracted with dichloromethane. The extract was washed with saturated brine, dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (petroleum ether/ethyl acetate) to give the title compound (1.10 g).

後処理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 2 hr
  3. extractionthe mixture was extracted with dichloromethane
  4. washThe extract was washed with saturated brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. customthe solvent was evaporated under reduced pressure
  7. customThe residue was purified by silica gel column chromatography (petroleum ether/ethyl acetate)

出典と根拠

ORDレコード
ord-c369f6431e194106ae6c8e3f9c3fa8c3
出典データセット
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09150588B2

反応ノート

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