反应详情

A mixture of 3-[3-(4-fluorophenyl)-1-[2-(4-fluorophenyl)-2-oxoethyl]-3-oxopropyl]-benzonitrile (1 g, 2.1 mmol), trimethylsilylazide (0.48 g, 4.2 mmol), and dibutyltin oxide (0.05 g) is heated under N2 in toluene (25 mL) at 100° C. for 18 hours. The toluene is removed under vacuum and the residue is dissolved in a small amount of methanol. The methanol is removed under vacuum and the residue chromatographed over SiO2 eluting with dichloromethane:2-propanol (4:1). Pure fractions are combined, concentrated, and triturated with diethyl ether to provide 0.8 g of the title compound; mp 162°-164C.

1. customThe toluene is removed under vacuum
2. dissolutionthe residue is dissolved in a small amount of methanol
3. customThe methanol is removed under vacuum
4. customthe residue chromatographed over SiO2 eluting with dichloromethane:2-propanol (4:1)
5. concentrationconcentrated
6. customtriturated with diethyl ether