Reaktion #538515

ord-4ded625ff5df4b219b6aa55c5b9ef778

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturAt 10° C.-30° C., with cooling
  2. 2
    Sonstigethe solvent is removed under reduced pressure at temperatures of down to 35° C

Vorschrift

To a solution of 100 g of ethyl 4-chloroacetoacetate in 300 ml of toluene and 100 ml of ethanol are added 6.7 ml of acetic acid. At 10° C.-30° C., with cooling, 47.4 g of isobutylamine are added dropwise. Subsequently, the mixture is stirred at room temperature for 8 h and the solvent is removed under reduced pressure at temperatures of down to 35° C. 140.8 g of ethyl 4-chloro-3-(isobutylamino)but-2-enecarboxylate are obtained in a purity of 79% (this corresponds to 86% yield).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08487112B2uspto-grants-2013_07