Réaction #86021

ord-bfb73c69bdd742a5a3bed3e647af96f8

Solvants

Conditions de réaction

Température
50°CELSIUS
Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    TempératureThe reaction mixture was cooled
  2. 2
    Extractionthe mixture was extracted with ethyl acetate
  3. 3
    Lavagethe extract was washed with saturated brine
  4. 4
    Séchagedried over anhydrous magnesium sulfate
  5. 5
    AutreThe solvent was evaporated under reduced pressure
  6. 6
    Autrepurification

Mode opératoire

A suspension of diethyl 2-benzyloxycarbonylaminomalonate (5.0 g), potassium carbonate (2.7 g), potassium iodide (0.32 g), and isopropyl 2-bromoacetate (3.5 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 (6.8 g, yield: 99%) as colorless oil.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US09434737B2uspto-grants-2016_09