反应详情

7-Nitro-1,2,4,5-tetrahydro-3H-3-benzazepine (1.1 g), 2-methanesulphonyloxyethyl azide (0.92 g) and potassium carbonate (0.76 g) were heated under reflux in acetonitrile for 18 hours. The solvent was evaporated in vacuo and the residue taken up in ethyl acetate then washed three times with aqueous sodium carbonate and three times with brine. The organic layer was dried, filtered and evaporated in vacuo to give an oil which was purified by chromatography on silica eluting with ethyl acetate/hexane (1:1). The product-containing fractions were combined and evaporated to give the title compound as an oil, yield 0.65 g, which was used without further purification.

1. customThe solvent was evaporated in vacuo
2. washthen washed three times with aqueous sodium carbonate and three times with brine
3. customThe organic layer was dried
4. filtrationfiltered
5. customevaporated in vacuo
6. customto give an oil which
7. customwas purified by chromatography on silica eluting with ethyl acetate/hexane (1:1)
8. customevaporated