Reaktion #8527

ord-3aa39437285a4e61ad16bed02546d92a

Reaktionsgleichung

[H][H]
hydrogen
Nc1ccc(F)c(F)c1F
2,3,4-Trifluoroaniline
COC(=O)C(C)=O
methyl pyruvate
O=S(=O)([O-])[O-].[Mg+2]
magnesium sulfate
COC(=O)C(C)Nc1ccc(F)c(F)c1F
title compound
Ausbeute 95.3%
COC(=O)C(C)Nc1ccc(F)c(F)c1F
Methyl 2-(2,3,4-trifluoroanilino)propionate
Ausbeute 95.3%

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
  3. 3
    SonstigeThe crystals thus precipitated
  4. 4
    Filtrationwere filtered
  5. 5
    Waschenwhile washing with hexane

Vorschrift

2,3,4-Trifluoroaniline (2.94 g) and methyl pyruvate (2.04 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 crystals thus precipitated were filtered while washing with hexane. Thus the title compound (4.44 g) was obtained as slightly yellowish crystals. Various spectral data of this product was identical with those obtained in Example 5.

Quelle

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