Reaktion #86022

ord-90797a7338924070b568b0d13d20c8a2

Lösungsmittel

Reaktionsbedingungen

Temperatur
50°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe reaction mixture was cooled
  2. 2
    Extraktionthe mixture was extracted with ethyl acetate
  3. 3
    Waschenthe extract was washed with saturated brine
  4. 4
    Trocknendried over anhydrous magnesium sulfate
  5. 5
    SonstigeThe solvent was evaporated under reduced pressure
  6. 6
    Sonstigepurification

Vorschrift

A suspension of diethyl 2-benzyloxycarbonylaminomalonate (5.0 g), potassium carbonate (2.7 g), potassium iodide (0.27 g), and t-butyl 2-bromoacetate (4.1 g) in DMF (50 mL) was stirred at 50° C. for 1 hour. The reaction mixture was cooled, and then poured into diluted hydrochloric acid, the mixture was extracted with ethyl acetate, and the extract was washed with saturated brine, and then dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure, and the residue was subjected to silica gel column chromatography, and then purification was performed with n-hexane/ethyl acetate (5:1), to obtain the title compound (6.9 g, yield: 99%) as colorless oil.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09434737B2uspto-grants-2016_09