반응 #89999

반응 방정식

Trifluoroacetic acid

8-(2-amino-ethoxy)-6,6-dimethyl-11-oxo-6,11-dihydro-5H-benzo[b]carbazole-3-carbonitrile

diisopropylethylamine

methanesulfonyl chloride

→

compound

수율 29.0%

N-[2-(3-Cyano-6,6-dimethyl-11-oxo-6,11-dihydro-5H-benzo[b]carbazol-8-yloxy)-ethyl]-methanesulfonamide

수율 29.0%

용매

water

dichloromethane

반응 조건

후처리

1. 1
   추출extracted with dichloromethane
2. 2
   세척After washing with saturated brine
3. 3
   건조the organic layer was dried over sodium sulfate
4. 4
   기타The drying agent was removed by filtration
5. 5
   기타the residues obtained
6. 6
   농축after concentration under reduced pressure
7. 7
   기타were separated by silica gel preparative TLC (ethyl acetate 100%)

실험 절차

Trifluoroacetic acid salt of 8-(2-amino-ethoxy)-6,6-dimethyl-11-oxo-6,11-dihydro-5H-benzo[b]carbazole-3-carbonitrile (Compound A8-2, 19 mg, 0.044 mmol) was suspended in dichloromethane (0.5 mL), added with diisopropylethylamine (0.0157 mL, 2 eq.) and methanesulfonyl chloride (0.0034 mL, 1 eq.), and then stirred at room temperature for 2 hr. The reaction solution was added to water, and then extracted with dichloromethane. After washing with saturated brine, the organic layer was dried over sodium sulfate. The drying agent was removed by filtration and the residues obtained after concentration under reduced pressure were separated by silica gel preparative TLC (ethyl acetate 100%) to obtain the target compound (5.5 mg, 29%).

출처