Hydrochloric Acid → 2-Chloro-1-(2,4-difluoro-5-methylphenyl)ethan-1-one

HRID 1784936

반응식

HRID 1784936 반응식
[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[CH3:9].[Al+3].[Cl-].[Cl-].[Cl-].[Cl:14][CH2:15][C:16](Cl)=[O:17].Cl>CCOC(C)=O.O>[Cl:14][CH2:15][C:16]([C:5]1[CH:4]=[C:3]([CH3:9])[C:2]([F:1])=[CH:7][C:6]=1[F:8])=[O:17]

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 6577Chloroacetyl chlorideHCID 679832,4-Difluoro-1-methylbenzeneHCID 6451240Aluminum(III) Chloride

생성물 1

HCID 739948662-Chloro-1-(2,4-difluoro-5-methylphenyl)ethan-1-one

시약·촉매·용매 2

HCID 962Water용매HCID 8857Ethyl Acetate용매

반응 조건

온도
0 °C

실험 절차

To a stirring solution of 2,4-difluorotoluene was added 6.3 g (47.3 mmol) of AlCl3, and 3.4 mL (42.6 mmol) of chloroacetyl chloride at 0° C. After the mixture was stirred for 10 min. at 0° C. and then at 45° C. for 30 min. The mixture was allowed to cool to r.t., about 16 mL of conc. HCl, 25 mL of water, and 100 mL of EtOAc were added. The organic layer was separated and washed with brine and sat. NaHCO3 (2×), and dried over Na2SO4. The solution was filtered and concentrated to give 9.0 g of 2-chloro-1-(2,4-difluoro-5-methylphenyl)ethanone as a colorless solid that was used without further purification.

후처리

  1. waitat 45° C. for 30 min
  2. temperatureto cool to r.t.
  3. customThe organic layer was separated
  4. washwashed with brine and sat. NaHCO3 (2×)
  5. dry with materialdried over Na2SO4
  6. filtrationThe solution was filtered
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-8235be2de36244b5931c0eec595e522e
출처 데이터셋
uspto-grants-2009_03
특허 번호
US07504420B2

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