Reaktion #54663

ord-1d94e2ec81454ab69745a7f772ddee44

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeAt the end of this time the ether layer was separated
  2. 2
    Trocknendried (MgSO4)
  3. 3
    SonstigeRemoval of the solvent
  4. 4
    workup.WAITleft an oily solid (12.3 g.)
  5. 5
    workup.DISTILLATIONThis was distilled under reduced pressure

Vorschrift

Sodium bicarbonate (8.4 g., 0.1 mole) and glycine ethyl ester hydrochloride (7 g. 0.05 mole) were dissolved in water (100 ml.), and a solution of p-menth-3-oyl chloride (10 g., 0.05 mole) in ether (50 ml.) was added and the mixture stirred vigorously at room temperature for 2 hours. At the end of this time the ether layer was separated and dried (MgSO4). Removal of the solvent left an oily solid (12.3 g.). This was distilled under reduced pressure to yield N-p-menth-3-oylglycine ethyl ester, bp. 150- 2°/0.1 mm. as a colourless liquid which rapidly solidified.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04150052uspto-grants-1979_04