反应详情

Hydrazine monohydrate (1.25 mi) and 8-chloro-10,11-dihydro-10[(1,3-dihydro-1,3-dioxo-2H-isoindol-2-yl)acetyl]-dibenz[b,f][1,4]-oxazepine (5.00 grams) were refluxed in absolute ethanol (125 mi) for 4 hours. The resulting mixture was filtered hot, and the collected solid was rinsed twice with ethanol, and then with hot methylene chloride. The filtrate and rinses were combined, evaporated i-n vacuo, and purified by flash chromatography through silica gel 60 (300 mi) using 95:5:0.5 chloroform:methanol:ammonium hydroxide. Trituration of the purified product with ethyl ether/hexane yielded the title compound as a white solid. Yield: 2.91 grams (84%). Mp: 108°-1090° C.

1. filtrationThe resulting mixture was filtered hot
2. washthe collected solid was rinsed twice with ethanol
3. customevaporated i-n vacuo
4. custompurified by flash chromatography through silica gel 60 (300 mi)