反应 #90159

ord-1fb2161f160e469688fad1ea50e74919

反应条件

温度
60°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

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

实验过程

9-Ethyl-6,6-dimethyl-11-oxo-8-(4-oxopiperidin-1-yl)-6,11-dihydro-5H-benzo[b]carbazole-3-carbonitrile (30 mg) and hydroxylamine hydrochloric acid salt (10 mg) were dissolved in ethanol (5 ml) and stirred at 60° C. for 6 hrs. The reaction mixture was diluted with ethyl acetate (20 ml). The organic layer was washed with 10% brine and 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 (23.5 mg, yield 74%).

来源

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