Reaktion #2362428

ord-c14ed9213fd14209abc26bc49f833c96

Reaktionsbedingungen

Temperatur
60°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Waschenthe organic layer was washed with 10% brine solution
  2. 2
    Einengenconcentrated under reduced pressure
  3. 3
    SonstigeThe resulting residues were purified by silica gel column (dichloromethane/methanol (=99/1))

Vorschrift

9-Ethyl-6,6-dimethyl-11-oxo-8-piperazin-1-yl-6,11-dihydro-5H-benzo[b]carbazole-3-carbonitrile (45 mg) and cyclohexanone (25 mg) were suspended in chloroform (2 ml), added with trimethylsilyl cyanide (30 mg) and zinc iodide (5 mg), and the mixture was stirred at 60° C. for 17 hrs. The reaction mixture was diluted with ethyl acetate (20 ml) and the organic layer was washed with 10% brine solution and concentrated under reduced pressure. The resulting residues were purified by silica gel column (dichloromethane/methanol (=99/1)) to obtain the title compound (12 mg, yield 30%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09126931B2uspto-grants-2015_09