反应详情

3-Bromo-9-((S)-2,2-dimethyl-[1,3]dioxolan-4-yl methoxy)-6,6-dimethyl-5,6-dihydro-benzo[b]carbazol-11-one (Compound JJ3-1, 49.5 mg, 0.105 mmol) and copper cyanide (90%, 35.3 mg, 3.4 eq.) were added with DMA (0.5 mL), and the mixture was irradiated with microwave at 200° C. for 1 hr under nitrogen atmosphere. After cooling, the reaction solution was added with water and extracted with ethyl acetate. The insoluble matters were separated off by filtration, and the organic layer was washed with brine and dried over magnesium sulfate. After filtration and the concentration under reduced pressure, the resulting residues were purified by preparative TLC (methanol/dichloromethane) to obtain the title compound (white solid, 8.5 mg, 22%).

1. customthe mixture was irradiated with microwave at 200° C. for 1 hr under nitrogen atmosphere
2. temperatureAfter cooling
3. extractionextracted with ethyl acetate
4. customThe insoluble matters were separated off by filtration
5. washthe organic layer was washed with brine
6. dry with materialdried over magnesium sulfate
7. filtrationAfter filtration
8. concentrationthe concentration under reduced pressure
9. customthe resulting residues were purified by preparative TLC (methanol/dichloromethane)