反应详情

To a solution of 2.58 g (10.0 mmol) of 3-methyl-1-[5-(amino)pentyl]-1,4,7b-triazacyclopent[cd]inden-2-one and 1.81 ml (13.0 mmol) of triethylamine in 100 ml of acetonitrile was added, while stirring under ice-cooling, 1.43 ml (12.0 mmol) of trifluoroacetic acid ethyl ester. The mixture was stirred for one hour at the same temperature. The solvent was distilled off. To the residue was added ethyl acetate—tetrahydrofuran. The mixture was washed with an aqueous saline solution, and dried over anhydrous magnesium sulfate. The solvent was distilled off. The residue was purified by column chromatography (eluent: ethyl acetate), which was recrystallized from ethyl acetate—n-hexane to afford 2.57 g (72.6%, a pale yellow crystals) of the desired compound.

1. temperaturecooling
2. stirringThe mixture was stirred for one hour at the same temperature
3. distillationThe solvent was distilled off
4. additionTo the residue was added ethyl acetate—tetrahydrofuran
5. washThe mixture was washed with an aqueous saline solution
6. dry with materialdried over anhydrous magnesium sulfate
7. distillationThe solvent was distilled off
8. customThe residue was purified by column chromatography (eluent: ethyl acetate), which
9. customwas recrystallized from ethyl acetate—n-hexane
10. customto afford 2.57 g (72.6%