反应 #90061

反应方程式

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

收率 194.9%

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

收率 194.9%

溶剂

NMP

反应条件

后处理

1. 1
   萃取extracted with ethyl acetate
2. 2
   洗涤The organic layer was washed with saturated brine
3. 3
   干燥dried over sodium sulfate
4. 4
   其他The drying agent was removed by filtration
5. 5
   其他the residues obtained
6. 6
   浓缩after concentration under reduced pressure
7. 7
   workup.ADDITIONwere added with MeOH
8. 8
   workup.DISSOLUTIONafter dissolution
9. 9
   过滤was filtered

实验过程

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%).

来源