反应详情

To a solution of 0.58 g (1.5 mM) of N-(piperidin-4-ylmethyl)-5-thia-1,8b-diazaacenaphthylene-4-carboxamide dihydrochloride and 1.0 ml (7.5 mM) of triethylamine in ethanol was added 0.19 ml (1.6 mM) of benzyl bromide at room temperature, and the mixture was refluxed under nitrogen for 6 hours. The solvent was then distilled off under reduced pressure and the residue was diluted with water and extracted with methylene chloride. The organic layer was washed with saturated aqueous solution of sodium chloride and dried over MgSO4. The resulting crude product was purified by column chromatography (methanol/ethyl acetate 40%) to provide the title compound.

1. temperaturethe mixture was refluxed under nitrogen for 6 hours
2. distillationThe solvent was then distilled off under reduced pressure
3. additionthe residue was diluted with water
4. extractionextracted with methylene chloride
5. washThe organic layer was washed with saturated aqueous solution of sodium chloride
6. dry with materialdried over MgSO4
7. customThe resulting crude product was purified by column chromatography (methanol/ethyl acetate 40%)