Hydrochloric Acid → 4,4,4-Trifluoro-1-(3-chloro-4-methoxylphenyl)-1,3-butanedione

HRID 1860583

반응식

HRID 1860583 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([C:10](=[O:12])[CH3:11])[CH:5]=[CH:6][C:7]=1[O:8][CH3:9].[F:13][C:14]([F:21])([F:20])[C:15](OCC)=[O:16].C[O-].[Na+].Cl>COCCOC.O.CCOC(C)=O>[F:13][C:14]([F:21])([F:20])[C:15](=[O:16])[CH2:11][C:10]([C:4]1[CH:5]=[CH:6][C:7]([O:8][CH3:9])=[C:2]([Cl:1])[CH:3]=1)=[O:12]

참가 물질

8

반응물 4

HCID 313Hydrochloric AcidHCID 9794Ethyl trifluoroacetateHCID 5208573'-Chloro-4'-methoxyacetophenoneHCID 10942334Sodium Methoxide

생성물 1

HCID 129727284,4,4-Trifluoro-1-(3-chloro-4-methoxylphenyl)-1,3-butanedione

시약·촉매·용매 3

HCID 962Water용매HCID 80711,2-Dimethoxyethane용매HCID 8857Ethyl Acetate용매

실험 절차

To stirred solution of 1-(3-chloro-4-methoxyphenyl)ethanone (2.2 g, 12 mmol) in DME was added ethyl trifluoroacetate (4.28 ml, 36 mmol) and sodium methoxide (4.25 g, 72 mmol), and the resulting reaction mixture was stirred at room temperature for 1 hour. EtOAc (200 ml) and water (50 ml) were added, and the pH of the aqueous layer was adjusted to 6 by addition of 1 N HCl solution. The organic layer was washed with brine (50 ml), dried over MgSO4, and concentrated in vacuo to give the title compound in quantitative yield. This was used for the next coupling step without further purification.

후처리

  1. customthe resulting reaction mixture
  2. washThe organic layer was washed with brine (50 ml)
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-bb16ff7b1ccb4c738b47374be0df0e0d
출처 데이터셋
uspto-grants-2003_03
특허 번호
US06531492B1

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