反应详情

To a suspension of 735 mg (4.24 mmol) of 1,2-dihydro-3-methyl-1,4,7b-triazacyclopent[cd]inden-2-one in 15 ml of DMF was added, while stirring under ice-cooling, 187 mg (4.68 mmol) of 60% sodium hydride (dispersion in oil). The mixture was stirred for 20 minutes at the same temperature. To the mixture was added a solution of 1.18 g (4.24 mmol) of 4-bromomethyl-1-tert-butoxycarbonylpiperidine in 5 ml of DMF. The mixture was stirred for one hour at 100° C. After cooling, the reaction mixture was poured into water and extracted with ethyl acetate. The extract was washed with water and brine, dried over anhydrous magnesium sulfate. The solvent was distilled off, and the residue was purified by column chromatography (eluent: ethyl acetate) to give 988 mg of the desired compound (62.8%, pale yellow solid).

1. additionwas added
2. temperaturecooling
3. stirringThe mixture was stirred for 20 minutes at the same temperature
4. stirringThe mixture was stirred for one hour at 100° C
5. temperatureAfter cooling
6. extractionextracted with ethyl acetate
7. washThe extract was washed with water and brine
8. dry with materialdried over anhydrous magnesium sulfate
9. distillationThe solvent was distilled off
10. customthe residue was purified by column chromatography (eluent: ethyl acetate)