反应详情

Combine 1-ethoxycarbonyl-4-(1H-benzimidazol-2-yl)[1,4]diazepane (16.7 g, 58 mmol) and aqueous 48% hydrobromic acid solution (80 mL). Heat to reflux. After 3 hours, cool to ambient temperature, add to ethanol (700 mL), and cool to 0° C. to give a solid. Combine the solid with aqueous 48% hydriodic acid (80 mL) and water (150 mL). Heat on a steam bath. After about 1 hour, cool to ambient temperature, dilute with ethanol (500 mL), and add to diethyl ether (8 L) to give a solid. Collect solid by filtration and dry in vacuo to give the title compound: mp; >290° C.

1. temperatureHeat to reflux
2. temperaturecool to 0° C.
3. customto give a solid
4. temperatureHeat on a steam bath
5. waitAfter about 1 hour
6. temperaturecool to ambient temperature
7. customto give a solid
8. customCollect solid
9. filtrationby filtration
10. customdry in vacuo