Reaktion #415548

ord-b414557362894aa4bce70175f46af473

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONis added simultaneously dropwise
  2. 2
    Sonstigethe product, (±)-2-acetylamino-2,3-dimethylbutyric acid, removed by filtration
  3. 3
    Waschenwashed with cold water
  4. 4
    Sonstigeair-dried
  5. 5
    SonstigeA sample recrystallized from acetonitrile

Vorschrift

To a stirred solution of 2-amino-2,3-dimethylbutyric acid (13.1 g) in 55 ml 2N NaOH maintained at 5° C is added simultaneously dropwise but separately 17 ml acetic anhydride and 95 ml 2N NaOH so that the pH of the solution is maintained at about 8.5. After stirring at room temperature for a further 1/2 hour, the mixture is acidified with concentrated HCl and the product, (±)-2-acetylamino-2,3-dimethylbutyric acid, removed by filtration, washed with cold water and air-dried. A sample recrystallized from acetonitrile had melting point 189°-190° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04017510uspto-grants-1977_04