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

HRID 579249
ノート
印刷プレビュー

反応式

HRID 579249 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収率 86.1%

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) (48.1 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) 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) acetate)

出典と根拠

ORDレコード
ord-1010ceadbac94158bd05e55250759a0f
出典データセット
uspto-grants-2015_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09040709B2

反応ノート

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