反応 #90156

ord-8606ccbc8cb34a6eac99f312a5237b9a

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    洗浄The organic layer was washed with 10% brine
  2. 2
    濃縮concentrated under reduced pressure
  3. 3
    その他The resulting residues were purified by silica gel column (dichloromethane/methanol=99/1 to 90/10)

実験手順

8-(1,4-Dioxa-8-aza-spiro[4.5]dec-8-yl)-9-ethyl-6,6-dimethyl-11-oxo-6,11-dihydro-5H-benzo[b]carbazole-3-carbonitrile, which had been prepared in Example 809, was dissolved in THF (10 ml), added with 5 N hydrochloric acid (50 ml), and the mixture was stirred for 17 hrs. The reaction mixture was neutralized with 5 N aqueous solution of sodium hydroxide and diluted with ethyl acetate (200 ml). The organic layer was washed with 10% brine, and then concentrated under reduced pressure. The resulting residues were purified by silica gel column (dichloromethane/methanol=99/1 to 90/10) to obtain the title compound (2.9 g, two step yield 64%).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US09440922B2uspto-grants-2016_09