Reaktion #466108

ord-175496a9e675424fb66852065d8ddadf

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturwas refluxed for 2 hours
  2. 2
    Temperaturto cool
  3. 3
    SonstigeA tan precipitate formed
  4. 4
    Temperaturupon cooling
  5. 5
    FiltrationThe solids were filtered off
  6. 6
    Sonstigethe filtrate was rotary evaporated
  7. 7
    Sonstigeto give a yellow gum
  8. 8
    Filtrationgravity filtered
  9. 9
    Temperaturto cool
  10. 10
    FiltrationThe resulting precipitate was filtered off
  11. 11
    Waschenwashed with water
  12. 12
    Sonstigedried in vacuo
  13. 13
    Sonstigeto give a yellow solid

Vorschrift

A stirred suspension of (±)-2-(acetylamino)-5-phenyl-pentanoic acid (0.5003 g, 0.002126 mol) in 2.8 M hydrochloric acid was refluxed for 2 hours, and the resulting brown solution was allowed to cool. A tan precipitate formed upon cooling. The solids were filtered off, and the filtrate was rotary evaporated to give a yellow gum. The gum was dissolved in hot water, gravity filtered, and allowed to cool. The mixture was made basic with 1 M sodium hydroxide to pH=5. The resulting precipitate was filtered off, washed with water, and dried in vacuo to give a yellow solid; yield 0.205 g (50%), mp=213-215° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06297247B1uspto-grants-2001_10