Ethanol → Ethyl 2-(2,3,4-trifluoroanilino)propionate

HRID 458163

反応式

HRID 458163 の反応式
[F:1][C:2]1[C:7]([F:8])=[C:6]([F:9])[CH:5]=[CH:4][C:3]=1[N+:10]([O-])=O.[C:13]([O:18][CH3:19])(=[O:17])[C:14]([CH3:16])=O.S([O-])([O-])(=O)=O.[Mg+2].[H][H].[CH2:28](O)C>[Pd].C(OCC)(=O)C.CCCCCC>[F:1][C:2]1[C:7]([F:8])=[C:6]([F:9])[CH:5]=[CH:4][C:3]=1[NH:10][CH:14]([CH3:16])[C:13]([O:18][CH2:19][CH3:28])=[O:17]

参加物

8

反応物 5

HCID 702EthanolHCID 11748Methyl pyruvateHCID 24083Sulfuric acid magnesium salt (1:1)HCID 698711,2,3-Trifluoro-4-nitrobenzeneHCID 178418361HCID 178418361、化合物

生成物 1

HCID 22015871Ethyl 2-(2,3,4-trifluoroanilino)propionate

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 21226206Ethyl acetate hexane溶媒

実験手順

2,3,4-Trifluoronitrobenzene (3.54 g) and methyl pyruvate (2.32 g) were dissolved in ethanol (30 ml). After adding 5% Pd—C (2.0 g) and anhydrous magnesium sulfate (2.65 g), the mixture was stirred at 50° C. in a hydrogen atmosphere for 16 hours. After filtering off Pd—C and magnesium sulfate, the obtained filtrate was concentrated under reduced pressure. The residue thus obtained was subjected to silica gel column chromatography (ethyl acetate-normal hexane=1:4) to give the title compound (4.84 g) as a pale yellow oily substance.

後処理

  1. filtrationAfter filtering off Pd—C and magnesium sulfate
  2. concentrationthe obtained filtrate was concentrated under reduced pressure
  3. customThe residue thus obtained

出典と根拠

ORDレコード
ord-24cc46561fb94f3180bc0dfdf92c9821
出典データセット
uspto-grants-2007_03
特許番号
US07189847B2

関連ノート

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