反应详情

A mixture of 2-nitro-10H-dibenzo[b,f][1,4]oxazepin-11-one (Example 3, 2.0 g, 7.8 mmol) and SnCl2 in 50 mL of denatured ethanol (85% ethanol, 15% wood alcohol) was stirred under reflux for 1 hr. The solvent was evaporated and the solid residue was washed with 200 mL of ethyl acetate. The ethyl acetate layer was washed with 1.0 N sodium hydroxide (2×100 mL)and water (2×100 mL), then dried over magnesium sulfate, filtered and evaporated to give an off white solid (yield 0.92 g, 52.3%).

1. temperatureunder reflux for 1 hr
2. customThe solvent was evaporated
3. washthe solid residue was washed with 200 mL of ethyl acetate
4. washThe ethyl acetate layer was washed with 1.0 N sodium hydroxide (2×100 mL)and water (2×100 mL)
5. dry with materialdried over magnesium sulfate
6. filtrationfiltered
7. customevaporated