반응 #90061

반응 방정식

NaOMe

1-dodecanethiol

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

hydrochloric acid

→

title compound

수율 194.9%

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

수율 194.9%

용매

NMP

반응 조건

후처리

1. 1
   추출extracted with ethyl acetate
2. 2
   세척The organic layer was washed with saturated brine
3. 3
   건조dried 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
   workup.ADDITIONwere added with MeOH
8. 8
   workup.DISSOLUTIONafter dissolution
9. 9
   여과was filtered

실험 절차

9-Bromo-8-methoxy-6,6-dimethyl-11-oxo-6,11-dihydro-5H-benzo[b]carbazole-3-carbonitrile (Compound E3-1-1, 1.0 g, 2.53 mmol) was dissolved in NMP (10 mL), added with NaOMe (683 mg, 5 eq.) and 1-dodecanethiol (3.0 mL, 5 eq.), and stirred at 160° C. for 1 hr. The reaction solution was added to 0.5 N aqueous solution of hydrochloric acid, and then extracted with ethyl acetate. The organic layer was washed with saturated brine and dried over sodium sulfate. The drying agent was removed by filtration and the residues obtained after concentration under reduced pressure were added with MeOH, and the solid remaining after dissolution was filtered to obtain the title compound (yellow powder, 1.88 g, 65%).

출처