反応 #90074

反応方程式

THF

9-acetyl-6,6-dimethyl-11-oxo-8-piperazin-1-yl-6,11-dihydro-5H-benzo[b]carbazole-3-carbonitrile

3-chloro-3-methyl-but-1-yne

triethylamine

→

title compound

収率 35.0%

9-Acetyl-8-[4-(1,1-dimethyl-prop-2-ynyl)-piperazin-1-yl]-6,6-dimethyl-11-oxo-6,11-dihydro-5H-benzo[b]carbazole-3-carbonitrile

収率 35.0%

溶媒

water

反応条件

後処理

1. 1
   抽出extracted with ethyl acetate
2. 2
   乾燥The organic layer was dried over magnesium sulfate
3. 3
   その他The drying agent was removed by filtration
4. 4
   その他the residues obtained
5. 5
   濃縮after concentration under reduced pressure
6. 6
   その他were purified by amino silica gel column chromatography (dichloromethane/methanol)

実験手順

To the anhydrous THF solution (0.5 mL) of 9-acetyl-6,6-dimethyl-11-oxo-8-piperazin-1-yl-6,11-dihydro-5H-benzo[b]carbazole-3-carbonitrile (Compound H8-5, 25 mg, 0.06 mmol), 3-chloro-3-methyl-but-1-yne (0.013 mL, 0.12 mmol), copper (I) chloride (0.6 mg, 0.006 mmol) and triethylamine (0.017 mL, 0.12 mmol) were added at room temperature. After stirring for 30 min, the mixture was added with water and extracted with ethyl acetate. The organic layer was dried over magnesium sulfate. The drying agent was removed by filtration and the residues obtained after concentration under reduced pressure were purified by amino silica gel column chromatography (dichloromethane/methanol) to obtain the title compound (white solid, 9.8 mg, 35%).

出典