反应详情

温度

50 °C

Under nitrogen atmosphere, 7-methoxy-6,6-dimethyl-11-oxo-6,11-dihydro-5H-benzo[b]carbazole-3-carbonitrile (Compound W3, 15 mg, 0.05 mmol) and triphenylphosphine (40 mg, 3 eq.) were added with THF (1 ml), further added dropwise with ((R)-2,2-dimethyl-[1,3]dioxolan-4-yl)-methanol (20 mg, 3 eq.) and 2.19 N toluene solution of diethyl azodicarboxylate (68 μL, 3 eq.), and the mixture was stirred at 50° C. for 2 hr. After cooling, the reaction solution was added with ethyl acetate, washed with brine, dried over sodium sulfate, and filtered. The residues obtained after concentration under reduced pressure were purified by preparative TLC (ethyl acetate/dichloromethane), and the resulting solid was washed with dichloromethane to obtain the target compound (brown powder, 5 mg).

1. temperatureAfter cooling
2. washwashed with brine
3. dry with materialdried over sodium sulfate
4. filtrationfiltered
5. customThe residues obtained
6. concentrationafter concentration under reduced pressure
7. customwere purified by preparative TLC (ethyl acetate/dichloromethane)
8. washthe resulting solid was washed with dichloromethane
9. customto obtain the target compound (brown powder, 5 mg)