Reaktion #416201

Reaktionsgleichung

water

Propargyl bromide

(±)-trans-1,2,3,4,4a,8,9,14a-octahydropyrido[4',3':2,3]indolo[1,7-ab][1]benzazepine

triethylamine

→

title compound

(±)-trans-1,2,3,4,4a,8,9,14a-octahydro-3-(2-propynyl)pyrido[4',3':2,3]indolo[1,7-ab][1]benzazepine

Lösungsmittel

DMF

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeSome precipitate had formed
2. 2
   SonstigeA solid precipitated which
3. 3
   Filtrationwas filtered off
4. 4
   Waschenwashed with cold water
5. 5
   SonstigeRecrystallization from 300 ml ethanol

Vorschrift

Propargyl bromide, 2.38 g, was added to a solution of (±)-trans-1,2,3,4,4a,8,9,14a-octahydropyrido[4',3':2,3]indolo[1,7-ab][1]benzazepine (5.52 g) and triethylamine (3ml) in 90 ml DMF. The reaction mixture was stirred at room temperature for 41/2 hours. Some precipitate had formed. The reaction mixture was poured into 300 ml of cold water. A solid precipitated which was filtered off and washed with cold water. Recrystallization from 300 ml ethanol gave 4.05 g of the title compound as pale yellow needles, m.p. 160°-161.5°. An analytical sample was recrystallized again from ethanol to give almost colorless needles, m.p. 162°-163° C.

Quelle