反应详情

A portion of the product from Step 1 (12.5 g, 48.6 mmol) was azeotroped with benzene and resuspended in benzene (94 mL). Et3N (9.49 mL, 68.1 mmol) and diphenylphosphoryl azide (10.48 mL, 48.6 mmol) were added, and the reaction mixture stirred at RT for 1 hour. The reaction mixture was then filtered through a pad of silica and eluted with ˜1 L of PhMe; the volatiles were evaporated; the residue was resuspended in diphenylmethane (94 mL); and the mixture heated to reflux for 3 hours (internal temperature 250° C.). The reaction mixture was allowed to cool to RT, stirred overnight, filtered and the solid washed with hexanes (100 mL) to give tan solid (7.4 g). LRMS ESI+ (M+H)+ 254.1.

1. filtrationThe reaction mixture was then filtered through a pad of silica
2. washeluted with ˜1 L of PhMe
3. customthe volatiles were evaporated
4. temperatureand the mixture heated
5. temperatureto reflux for 3 hours (internal temperature 250° C.)
6. temperatureto cool to RT
7. stirringstirred overnight
8. filtrationfiltered
9. washthe solid washed with hexanes (100 mL)