反应详情

温度

80 °C

Sodium azide (3.07 g, 0.047 mol) was added to a solution of 1 (12.9 g, 0.04 mol) in anhydrous DMF (70 mL) and the reaction mixture was stirred 12 h at 80° C. (oil bath). Then solvent was removed at reduced pressure and the residual oil was treated with a mixture of CH2Cl2/ether 3:1 (100 mL). The resulting solution was washed with water (2×100 mL), brine and dried over magnesium sulfate. The solvent was removed under reduced pressure and 7.6 g (95%) of 2 was obtained. The purity of 2 (99%) was determined by GC and TLC (eluent:hexane/ethyl acetate 1:1), Rf=0.84.

1. customThen solvent was removed at reduced pressure
2. additionthe residual oil was treated with a mixture of CH2Cl2/ether 3:1 (100 mL)
3. washThe resulting solution was washed with water (2×100 mL), brine
4. dry with materialdried over magnesium sulfate
5. customThe solvent was removed under reduced pressure