Реакция #90061

Уравнение реакции

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

Выход 194.9%

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

Выход 194.9%

Растворители

NMP

Условия реакции

Обработка

1. 1
   Экстракцияextracted with ethyl acetate
2. 2
   ПромывкаThe organic layer was washed with saturated brine
3. 3
   Сушкаdried over sodium sulfate
4. 4
   ДругоеThe drying agent was removed by filtration
5. 5
   Другоеthe residues obtained
6. 6
   Концентрированиеafter concentration under reduced pressure
7. 7
   workup.ADDITIONwere added with MeOH
8. 8
   workup.DISSOLUTIONafter dissolution
9. 9
   Фильтрацияwas filtered

Методика

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%).

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