Reaktion #416200

ord-056e9fa4c4734dc388454b9a3f610f02

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeSolution resulted immediately
  2. 2
    Sonstigehad formed
  3. 3
    Sonstigea gummy solid was separated
  4. 4
    Waschenwashed by decantation with cold water
  5. 5
    SonstigeRecrystallization from ethanol

Vorschrift

A suspension of 2.76 g of (±)-trans-1,2,3,4,4a,8,9,14a-octahydropyrido[4',3';2,3]indolo[1,7-ab][1]benzazepine in 20 ml of dimethylformamide (DMF) containing 2.3 ml triethylamine was treated with 1.25 g of 1,3-dichloro-2-butene. Solution resulted immediately. The solution was stirred at room temperature for 4 hours, by which time some white precipitate had formed. The reaction mixture was poured into 150 ml of cold water, a gummy solid was separated and washed by decantation with cold water. Recrystallization from ethanol gave 2.93 g of the title compound, m.p. 130°-132° C.

Quelle

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