反应详情

Combine 1-ethoxycarbonyl-4-(1H-benzimidazol-2-yl)[1,4]diazepane (5.22 g, 18.1 mmol) and aqueous 48% hydrobromic acid solution (25 mL). Heat to reflux. After 4 hours, cool to ambient temperature and concentrate in vacuo to give a residue. Combine the residue and ethanol (150 mL). Evaporate in vacuo to a volume of about 75 mL and cool to give a solid. Collect solid by filtration, rinse with ethanol and then diethyl ether, and dry in vacuo to give 4-(1H-benzimidazol-2-yl)[1,4 ]diazepane hydrobromic acid salt. Elemental Analysis calculated for C12H16N4•2HBr: C, 38.12; H, 4.80; N, 14.82. Found: C, 38.17; H, 4.84; N, 14.60.

1. temperatureHeat to reflux
2. concentrationconcentrate in vacuo
3. customto give a residue
4. customEvaporate in vacuo to a volume of about 75 mL
5. temperaturecool
6. customto give a solid
7. customCollect solid
8. filtrationby filtration
9. washrinse with ethanol
10. dry with materialdiethyl ether, and dry in vacuo