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Ethanol → 1-(4-Fluorophenyl)-2-(methylsulfonyl)-1-ethanone

HRID 335435
ノート
印刷プレビュー

反応式

HRID 335435 の反応式
[CH3:1][S:2]([O-:4])=[O:3].[Na+].[F:6][C:7]1[CH:16]=[CH:15][C:10]([C:11](=[O:14])[CH2:12]Cl)=[CH:9][CH:8]=1.C(O)C>O>[F:6][C:7]1[CH:16]=[CH:15][C:10]([C:11](=[O:14])[CH2:12][S:2]([CH3:1])(=[O:4])=[O:3])=[CH:9][CH:8]=1
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 702EthanolHCID 1202482-Chloro-4'-fluoroacetophenoneHCID 2733271Sodium methanesulfinate

生成物 1

HCID 14882461-(4-Fluorophenyl)-2-(methylsulfonyl)-1-ethanone

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a 1 L volume four-necked flask, sodium methanesulfinate (31.3 g), 4-fluorophenacyl chloride (21-b) (4.8.1 g), and ethanol (300 ml) were added under a nitrogen atmosphere, and heated to reflux for 1 hour. After the mixture was cooled to room temperature, water (500 ml) was added. The precipitated solids were collected by filtration, washed with water, and dried. The solids were dissolved in ethyl acetate, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The resulting residue was purified by recrystallization (hexane-ethyl acetate) to give 51.9 g of 1-(4-fluorophenyl)-2-methylsulfonylethan-1-one (7-2-3).

後処理

  1. temperatureheated
  2. temperatureto reflux for 1 hour
  3. filtrationThe precipitated solids were collected by filtration
  4. washwashed with water
  5. customdried
  6. dissolutionThe solids were dissolved in ethyl acetate
  7. dry with materialdried over anhydrous sodium sulfate
  8. concentrationconcentrated under reduced pressure
  9. customThe resulting residue was purified by recrystallization (hexane-ethyl acetate)

出典と根拠

ORDレコード
ord-d69d6367ce7c4a9f8ee96be6fab9bc96
出典データセット
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08884010B2

反応ノート

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