反应详情

温度

60 °C

2.0 g of sodium azide were added to 20 ml of dimethylformamide containing 1.6 g of 3-bromo-6-phenylperhydroazepin-2-one (Isomer A) [prepared as described in step (e) above]. The mixture was stirred for 6 hours at 60° C. and then diluted with ethyl acetate, washed with water three times and dried over anhydrous magnesium sulfate. The solvent was then distilled off. The crystalline residue was triturated in a 1:1 by volume mixture of methylene chloride and diisopropyl ether and then collected by filtration, to give 1.14 g of the title compound melting at 150°-152° C. (with decomposition).

1. custom[prepared as described in step (e) above]
2. washwashed with water three times
3. dry with materialdried over anhydrous magnesium sulfate
4. distillationThe solvent was then distilled off
5. customThe crystalline residue was triturated in a 1:1 by volume mixture of methylene chloride and diisopropyl ether
6. filtrationcollected by filtration