反应详情

温度

90 °C

To the ethanol (8 ml) suspension of 4-(6,6-dimethyl-2-nitro-11-oxo-6,11-dihydro-5H-benzo[b]carbazole-8-yl oxy)-piperidine-1-carboxylic acid tert-butyl ester (Compound P4, 103 mg, 0.204 mmol), iron powder (228 mg, 20 eq.), ammonium chloride (109 mg, 10 eq.), and distilled water (4 ml) were added and the mixture was stirred at 90° C. for 30 min. Upon the completion of the reaction, insoluble matters were filtered off, and the filtrate was extracted with ethyl acetate. The organic layer was washed with brine and dried over sodium 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 title compound (115 mg, 57%).

1. distillationdistilled water (4 ml)
2. additionwere added
3. customUpon the completion of the reaction, insoluble matters
4. filtrationwere filtered off
5. extractionthe filtrate was extracted with ethyl acetate
6. washThe organic layer was washed with brine
7. dry with materialdried over sodium sulfate
8. customThe drying agent was removed by filtration
9. customthe residues obtained
10. concentrationafter concentration under reduced pressure
11. customwere purified by silica gel column chromatography (ethyl acetate/hexane)