Reaktion #8529

ord-c97f457d75724fd29a32be088e5f8a4c

Reaktionsgleichung

[H][H]
hydrogen
Nc1ccc(F)c(F)c1F
2,3, 4-Trifluoroaniline
CCOC(=O)C(C)=O
ethyl pyruvate
O=S(=O)([O-])[O-].[Mg+2]
magnesium sulfate
CCOC(=O)C(C)Nc1ccc(F)c(F)c1F
title compound
Ausbeute 95.0%
CCOC(=O)C(C)Nc1ccc(F)c(F)c1F
Ethyl 2-(2,3,4-trifluoroanilino)propionate
Ausbeute 95.0%

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

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

Vorschrift

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.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07087778B2uspto-grants-2006_08