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

HRID 8433

반응식

HRID 8433 반응식
[F:1][C:2]1[C:8]([F:9])=[C:7]([F:10])[CH:6]=[CH:5][C:3]=1[NH2:4].[C:11]([O:16][CH2:17][CH3:18])(=[O:15])[C:12]([CH3:14])=O.S([O-])([O-])(=O)=O.[Mg+2].[H][H]>CO.[Pd]>[F:1][C:2]1[C:8]([F:9])=[C:7]([F:10])[CH:6]=[CH:5][C:3]=1[NH:4][CH:12]([CH3:14])[C:11]([O:16][CH2:17][CH3:18])=[O:15]

참가 물질

7

반응물 4

HCID 12041Ethyl pyruvateHCID 24083Sulfuric acid magnesium salt (1:1)HCID 774682,3,4-TrifluoroanilineHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 22015871Ethyl 2-(2,3,4-trifluoroanilino)propionate수율 95%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

2,3, 4-Trifluoroaniline (2.94 g) and ethyl pyruvate (2.32 g) were dissolved in methanol (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 obtained residue was subjected to silica gel column chromatography (ethyl acetate-normal hexane=1:4) to thereby give the title compound (4.69 g) as a pale yellow oily substance. Various spectral data of this product was identical with those obtained in Example 7.

후처리

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

출처 및 근거

ORD 기록
ord-c97f457d75724fd29a32be088e5f8a4c
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07087778B2

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