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

HRID 231122

반응식

HRID 231122 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-c62facb23d654e3e81f07915e4d8f847
출처 데이터셋
uspto-grants-1989_07
특허 번호
US04845116

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