Reaktion #342580

ord-60f8f45313854275aba8a55ac21693a9

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeTo a 1 liter, four-necked flask equipped with nitrogen inlet
  2. 2
    workup.ADDITIONwas added
  3. 3
    WaschenThe reaction mixture was washed with hexane
  4. 4
    Sonstigethe resulting solid was dried in vacuo

Vorschrift

To a 1 liter, four-necked flask equipped with nitrogen inlet, thermometer, and mechanical stirrer was charged 499.74 g (490 ml, 3.84 mol) of ethyl acetoacetate and 12.9 g (0.115 mol) of potassium-t-butoxide. The resulting mixture was stirred while 391 g (4.04 mol) of trifluoroaceto-nitrile was added. The reaction mixture was washed with hexane and the resulting solid was dried in vacuo affording 535 g (62%) of the enamine as a yellow solid; mp 63°-65° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04698093uspto-grants-1987_10