反应详情

A mixture of 1H-benzimidazol-2-yl(3-bromophenyl)methanol (12.9 g), 4-hydroxy-1-methylpiperidine (4.86 g) and para-toluenesulfonic acid (24 g) in chlorobenzene (60 mL) and N-methylpyrrolidone (6 mL) is heated under reflux for 120 h in a Dean Stark apparatus. Solvent is removed by evaporation. To the residue is added water which is made alcaline by addition of sodium hydroxide solution, then extracted with ethyl acetate. The pooled organic extracts are washed with water, treated with activated charcoal, dried over magnesium sulfate and concentrated under reduced pressure. The residue is triturated in diethyl ether to give 2-[(3-bromophenyl)(1-methylpiperidin-4-yloxy)methyl]-1H-benzimidazole.

1. temperatureis heated
2. temperatureunder reflux for 120 h in a Dean Stark apparatus
3. customSolvent is removed by evaporation
4. additionTo the residue is added water which
5. additionby addition of sodium hydroxide solution
6. extractionextracted with ethyl acetate
7. washThe pooled organic extracts are washed with water
8. additiontreated with activated charcoal
9. dry with materialdried over magnesium sulfate
10. concentrationconcentrated under reduced pressure
11. customThe residue is triturated in diethyl ether