反应详情

A solution of 9 (11.5 g, 31.8 mmol) and sodium azide (4.12 g, 64 mmol) in 250 ml of DMF was heated to 70° C. for 24 hours. After cooling to room temperature the solvent was removed in vacuo and the residue partitioned between chloroform and water. The organics were dried over MgSO4, filtered and the solvent removed in vacuo. The crude product was purified by chromatography on silica gel (8:1 hexane: ethyl acetate) afforded the title compound.

1. customwas removed in vacuo
2. customthe residue partitioned between chloroform and water
3. dry with materialThe organics were dried over MgSO4
4. filtrationfiltered
5. customthe solvent removed in vacuo
6. customThe crude product was purified by chromatography on silica gel (8:1 hexane: ethyl acetate)