反应详情

Combine (1-(4-fluorobenzyl)-1H-benzimidazol-2-yl)-(1-ethoxycarbonyl-piperidin-4-yl)amine (31.5 g, 79.4 mmol) and 48% hydrobromic acid (250 mL). Heat to reflux. After 1.5 hours, cool and evaporate in vacuo to give a residue. Add water and sodium hydroxide (60 g) and extract with chloroform. Dry the organic layer over Na2SO4, filter, and concentrate in vacuo to obtain a solid. Collect the solid by filtration and recrystallize from hexane/chloroform to give, after drying, the title compound: mp; 212-215° C.

1. temperatureHeat to reflux
2. temperaturecool
3. customevaporate in vacuo
4. customto give a residue
5. extractionAdd water and sodium hydroxide (60 g) and extract with chloroform
6. dry with materialDry the organic layer over Na2SO4
7. filtrationfilter
8. concentrationconcentrate in vacuo
9. customto obtain a solid
10. customCollect the solid
11. filtrationby filtration
12. customrecrystallize from hexane/chloroform
13. customto give
14. customafter drying