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Isopropanol → 4-Bromo-3-chloro-3,4,4-trifluorobutanoic acid

HRID 945
ノート
印刷プレビュー

反応式

HRID 945 の反応式
[Br:1][C:2]([F:10])([F:9])[C:3]([Cl:8])([F:7])[CH2:4][CH2:5][OH:6].CC(C)=[O:13].OS(O)(=O)=O.O=[Cr](=O)=O.C(O)(C)C>CC(C)=O.C(Cl)Cl>[Br:1][C:2]([F:10])([F:9])[C:3]([Cl:8])([F:7])[CH2:4][C:5]([OH:13])=[O:6]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 3776IsopropanolHCID 218364774-Bromo-3-chloro-3,4,4-trifluorobutan-1-olHCID 131709961Jones' reagent

生成物 1

HCID 109121274-Bromo-3-chloro-3,4,4-trifluorobutanoic acid収率 85%

試薬・触媒・溶媒 2

HCID 180Acetone溶媒HCID 6344Dichloromethane溶媒
このページの内容参加物実験手順後処理出典と根拠反応ノート

実験手順

A solution of 4-bromo-3-chloro-3,4,4-trifluorobutanol (IX) (2.41 g, 10 mmol) in acetone (35 mL) was treated with Jones reagent (7.5 mL) in 10 min with stirring and cooling (ice-water bath). The mixture was then stirred at room temperature for 30 min and 0.5 mL of i-propanol was then added. The precipitated salts were removed by filtration, washed with acetone. The residue obtained after concentration of the flitrate was dissolved in methylene chloride (100 mL), washed with 1N HCl (50 mL), brine, and dried over anhydrous magnesinm sulfate. Evaporation of the solvent gave 2.17 g (85%) of 4-bromo-3-chloro-3,4,4-trifluorobutanoic acid (VIII) as a clear oil.

後処理

  1. stirringThe mixture was then stirred at room temperature for 30 min
  2. customThe precipitated salts were removed by filtration
  3. washwashed with acetone
  4. customThe residue obtained after concentration of the flitrate
  5. washwashed with 1N HCl (50 mL), brine
  6. dry with materialdried over anhydrous magnesinm sulfate
  7. customEvaporation of the solvent

出典と根拠

ORDレコード
ord-cc001eb75d5743259d85df36a16ea38b
出典データセット
uspto-grants-1998_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05723470

反応ノート

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