Reaktion #1921687

ord-64c5fa1a42834066903cd982313e3100

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe resulting mixture was then heated for 1 hour
  2. 2
    Temperaturat reflux
  3. 3
    Temperaturcooled
  4. 4
    SonstigeThe ether solution was decanted from the inorganic salts
  5. 5
    Trocknendried over anhydrous potassium carbonate
  6. 6
    Sonstigeevaporated
  7. 7
    SonstigeThe solid residue thus obtained
  8. 8
    Sonstigewas recrystallized from benzene-hexane

Vorschrift

1.5 grams (0.036 moles) of (±)-trans-1,2,3,4,4a,8,9,14a-octahydropyrido[4',3':2,3]indolo[1,7-ab][1]benzazepine-3-hexanoic acid ethyl ester dissolved in 25 ml of dry ether was added dropwise to a stirred suspension of 380 mg (0.010 moles) of lithium aluminum hydride in 50 ml of ether under a nitrogen atmosphere. The resulting mixture was then heated for 1 hour at reflux, cooled, and decomposed with 1N sodium hydroxide solution. The ether solution was decanted from the inorganic salts, dried over anhydrous potassium carbonate, and evaporated. The solid residue thus obtained was recrystallized from benzene-hexane to give the title compound as colorless plates, m.p. 101°-102.5° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04070467uspto-grants-1978_01