Reaktion #1829657

ord-fb684e7ea37a4e908e14c1043ecb02eb

Lösungsmittel

Reaktionsbedingungen

Temperatur
0°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONis added to the reaction mixture which
  2. 2
    Filtrationthe suspension is filtered

Vorschrift

18 g of sodium hydroxide are dissolved in 250 ml of methanol and 75 g of p-hydroxy-phenyl-glycine are added. After stirring at 60° C. for 15 minutes 2 ml of acetic acid is added to the reaction mixture which is cooled to 0° C. and the suspension is filtered. The wet p-hydroxy-phenyl-glycine sodium salt obtained is suspended in 500 ml of ethanol, 75 g of acetoacetic acid methylester and 0.5 ml of acetic acid are added and the mixture is refluxed for 90 minutes. The residue is cooled to -5° C. and the suspension obtained is filtered, the crystals are dried in vacuo at 60° C. 124.1 g of sodium-D-N-(2-methoxy-carbonyl-1-methyl-vinyl)-α-amino-(p-hydroxy-phenyl)-acetate are obtained.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05338868uspto-grants-1994_08