Reaktion #49167

ord-52b52b1c24a64847a3cd38a59d3ea0ba

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigewas ascertained by TLC (19 h)
  2. 2
    SonstigeAfter 19 h which it was partitioned with dichloromethane (3×100 mL)
  3. 3
    TrocknenThe organic layer was dried with anhydrous sodium sulfate
  4. 4
    Filtrationfiltered
  5. 5
    Sonstigeevaporated
  6. 6
    workup.DISTILLATIONThe residue was distilled
  7. 7
    Sonstigeto afford AA (28.8 g, 61%)

Vorschrift

A 4.7M aqueous solution of sodium hydroxide (50 mL) was added into a stirred, ice-cooled solution of ethyl glycinate hydrochloride (32.19 g, 0.23 mole) in water (50 mL). Then, ethyl acrylate (23.1 g, 0.23 mole) was added and the mixture was stirred at room temperature until the completion of reaction was ascertained by TLC (19 h). After 19 h which it was partitioned with dichloromethane (3×100 mL). The organic layer was dried with anhydrous sodium sulfate, filtered and evaporated. The residue was distilled to afford AA (28.8 g, 61%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07745608B2uspto-grants-2010_06