反应详情

温度

140 °C

N-(2-Cyano-3-cyclopropylphenyl)-benzenesulfonamide (Intermediate 9, 0.052 g), azidotrimethyl-silane (0.087 g) and dibutyltin oxide (0.038 g) were suspended in 1,2-dichloroethane (3 mL). The mixture was heated by microwave irradiation at 140° C. for 45 minutes. Six further aliquots of azidotrimethylsilane (0.174 g) were added and after each addition the mixture was heated by microwave irradiation at 140° C. for 60 minutes. The reaction mixture was acidified to pH 1 using 1N hydrochloric acid, and then extracted with ethyl acetate. The combined organic extracts were dried with magnesium sulfate, filtered and the filtrate was evaporated under vacuum. The residue was triturated with a mixture of pentane and cyclohexane and the solid was collected by filtration, to give the title compound as a white solid (0.039 g).

1. additionafter each addition the mixture
2. temperaturewas heated by microwave irradiation at 140° C. for 60 minutes
3. extractionextracted with ethyl acetate
4. dry with materialThe combined organic extracts were dried with magnesium sulfate
5. filtrationfiltered
6. customthe filtrate was evaporated under vacuum
7. customThe residue was triturated with a mixture of pentane and cyclohexane
8. filtrationthe solid was collected by filtration