1,3-Difluorobenzene → 4-Chloro-1-(2,4-difluorophenyl)butan-1-one

HRID 231122

反応式

HRID 231122 の反応式
[Cl:1][CH2:2][CH2:3][CH2:4][C:5](Cl)=[O:6].[F:8][C:9]1[CH:14]=[CH:13][CH:12]=[C:11]([F:15])[CH:10]=1.[Cl-].[Al+3].[Cl-].[Cl-]>C(Cl)Cl>[Cl:1][CH2:2][CH2:3][CH2:4][C:5]([C:12]1[CH:13]=[CH:14][C:9]([F:8])=[CH:10][C:11]=1[F:15])=[O:6]

参加物

5

反応物 3

HCID 97411,3-DifluorobenzeneHCID 783704-Chlorobutyryl chlorideHCID 6451240Aluminum(III) Chloride

生成物 1

HCID 103310104-Chloro-1-(2,4-difluorophenyl)butan-1-one収率 85.2%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

255 g (1.81 mols) of 4-chlorobutyryl chloride are added dropwise to a mixture of 200 g (1.75 mols) of 1,3-difluorobenzene and 256 g (1.92 mols) of anhydrous aluminum chloride at room temperature, while stirring. The mixture is stirred at 30° C. for 4 hours and then poured onto 1,200 g of ice. 1,200 ml of methylene chloride are added, the organic phase is separated off, the aqueous phase is extracted with methylene chloride and the combined organic phases are washed with water, dried over sodium sulphate and concentrated by stripping off the solvent under reduced pressure. The residue which remains is distilled. 326 g (85% of theory) of 2,4-difluorophenyl 3-chloropropyl ketone are obtained in this manner.

後処理

  1. stirringThe mixture is stirred at 30° C. for 4 hours
  2. customthe organic phase is separated off
  3. extractionthe aqueous phase is extracted with methylene chloride
  4. washthe combined organic phases are washed with water
  5. dry with materialdried over sodium sulphate
  6. concentrationconcentrated
  7. distillationThe residue which remains is distilled

出典と根拠

ORDレコード
ord-c62facb23d654e3e81f07915e4d8f847
出典データセット
uspto-grants-1989_07
特許番号
US04845116

関連ノート

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