반응 #90009

반응 방정식

water

8-Hydroxy-6,6-dimethyl-11-oxo-6,11-dihydro-5H-benzo[b]carbazole-3-carbonitrile

Compound A6

8-Hydroxy-6,6-dimethyl-11-oxo-6,11-dihydro-5H-benzo[b]carbazole-3-carbonitrile

trifluoromethanesulfonic acid

→

Trifluoro-methanesulfonic acid 3-cyano-6,6-dimethyl-11-oxo-6,11-dihydro-5H-benzo[b]carbazol-8-yl ester

용매

pyridine

반응 조건

후처리

1. 1
   추출extracted with dichloromethane
2. 2
   건조The organic layer was dried over magnesium sulfate
3. 3
   기타The drying agent was removed by filtration
4. 4
   기타the residues obtained
5. 5
   농축after concentration under reduced pressure
6. 6
   기타were purified by silica gel column chromatography (ethyl acetate/hexane)
7. 7
   기타to obtain the target compound (white powder, 641 mg, 81%)

실험 절차

8-Hydroxy-6,6-dimethyl-11-oxo-6,11-dihydro-5H-benzo[b]carbazole-3-carbonitrile (Compound A6, 550 mg, 0.189 mmol) was dissolved in pyridine (18 mL), added with anhydrous trifluoromethanesulfonic acid (0.758 ml, 3 eq.), and stirred at room temperature for 30 min. The reaction solution was added to water and then extracted with dichloromethane. 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 silica gel column chromatography (ethyl acetate/hexane) to obtain the target compound (white powder, 641 mg, 81%).

출처