반응 #90148

ord-f2f7d8e5a65e478fb48d3610106645e5

반응 조건

온도
60°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

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

실험 절차

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%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09440922B2uspto-grants-2016_09