反应详情

温度

50 °C

Under nitrogen atmosphere, 9-bromo-3-chloro-8-hydroxy-6,6-dimethyl-5,6-dihydro-benzo[b]carbazol-11-one (Compound S2-4, 76 mg, 0.2 mmol) and triphenylphosphine (69 mg, 1.3 eq.) were added with THF (2 ml), and ((S)-2,2-dimethyl-[1,3]dioxolan-4-yl)-methanol (35 mg, 1.3 eq.) and 2.19 N toluene solution (118 μL, 1.3 eq.) of diethyl azodicarboxylic acid were added dropwise thereto, followed by stirring 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 silica gel column chromatography (ethyl acetate/dichloromethane) to give a solid, which was then washed with dichloromethane to obtain the title compound (brown powder, 53 mg).

1. additionwere added dropwise
2. temperatureAfter cooling
3. washwashed with brine
4. dry with materialdried over sodium sulfate
5. filtrationfiltered
6. customThe residues obtained
7. concentrationafter concentration under reduced pressure
8. customwere purified by silica gel column chromatography (ethyl acetate/dichloromethane)
9. customto give a solid, which
10. washwas then washed with dichloromethane