Reaktion #416203

ord-26158a1e72fa4421acd3e10164e0b61a

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.WAITto stand at room temperature for three days
  2. 2
    Filtrationwas then filtered
  3. 3
    Sonstigeevaporated to dryness in vacuo
  4. 4
    Sonstigetriturated with pentane
  5. 5
    SonstigeThe resulting solid was recrystallized from ethanol

Vorschrift

2.3 grams of methyl vinyl ketone was added to a solution of 8.3 grams of (±)-trans-1,2,3,4,4a,8,9,14a-octahydropyrido[4',3':2,3]indolo[1,7-ab][1]benzazepine in 400 ml. of ethanol. The mixture was permitted to stand at room temperature for four days, after which an additional 2.6 grams of methyl vinyl ketone was added. This mixture was permitted to stand at room temperature for three days, and was then filtered, evaporated to dryness in vacuo, and triturated with pentane. The resulting solid was recrystallized from ethanol to yield 9 grams of the title compound with m.p. 102.5° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04018930uspto-grants-1977_04