反应详情

A mixture of the compound of Example 1 (2.80 g, 5.52 mmol) and lithium azide (0.41 g, 8.28 mmol) in 30 ml of DMF is heated to 75°-80° (oil bath) for 2 h. The solvent is evaporated to dryness under reduced pressure. The residue is coevaporated several times with ethanol and triturated with ether. The white solid is collected by filtration, washed with ice-cooled water, a small amount of ethanol and ether, and then dried under reduced pressure to afford 1.35 g (65%) of the desired product. An analytical sample is obtained by recrystallization from 95% ethanol; mp 185°-186° (dec); ir (KBr): 4.78 λ (azido).

1. temperatureis heated to 75°-80° (oil bath) for 2 h
2. customThe solvent is evaporated to dryness under reduced pressure
3. customtriturated with ether
4. filtrationThe white solid is collected by filtration
5. washwashed with ice-
6. temperaturecooled water
7. dry with materiala small amount of ethanol and ether, and then dried under reduced pressure