反応 #90159

反応方程式

9-Ethyl-6,6-dimethyl-11-oxo-8-(4-oxopiperidin-1-yl)-6,11-dihydro-5H-benzo[b]carbazole-3-carbonitrile

hydroxylamine hydrochloric acid salt

→

title compound

収率 75.6%

9-Ethyl-8-(4-hydroxyimino-piperidin-1-yl)-6,6-dimethyl-11-oxo-6,11-dihydro-5H-benzo[b]carbazole-3-carbonitrile

収率 75.6%

溶媒

ethyl acetate

ethanol

反応条件

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

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%).

出典