反应详情

温度

57.5 °C

A solution of crude mesylate 1 (90.0 g, 0.495 mol) in DMF (500 mL) was treated with NaN3 (48.22g, 0.74 mol, 1.5 equiv) at 25° C. under N2. The resulting reaction mixture was warmed to 55-60° C. for 6-8 h with stirring before being quenched with H2O (500 mL). The pale-yellow solution was then extracted with EtOAc or Et2O (4×200 mL). The combined EtOAc (or Et2O) extracts were washed with H2O (3×500 mL), dried (MgSO4), and concentrated in vacuo. The residual solution was found to contain desired azide 2 (60.3 g, 64.5 g theoretical, 94%), which was found to be pure enough and directly used in the following reaction without further purification.

1. customThe resulting reaction mixture
2. custombefore being quenched with H2O (500 mL)
3. extractionThe pale-yellow solution was then extracted with EtOAc or Et2O (4×200 mL)
4. washThe combined EtOAc (or Et2O) extracts were washed with H2O (3×500 mL)
5. dry with materialdried (MgSO4)
6. concentrationconcentrated in vacuo
7. customdirectly used in the following reaction without further purification