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

HRID 458163

반응식

HRID 458163 반응식
[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]

참가 물질

8

반응물 5

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

생성물 1

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

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 21226206Ethyl acetate hexane용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-24cc46561fb94f3180bc0dfdf92c9821
출처 데이터셋
uspto-grants-2007_03
특허 번호
US07189847B2

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