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

HRID 1860583

反応式

HRID 1860583 の反応式
[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]

参加物

8

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 80711,2-Dimethoxyethane溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-bb16ff7b1ccb4c738b47374be0df0e0d
出典データセット
uspto-grants-2003_03
特許番号
US06531492B1

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