反应详情

To a suspension of 8.66 g (50 mmol) of 1,2-dihydro-3-methyl-1,4,7b-triazacyclopent[cd]inden-2-one in 100 ml of DMF was added, while stirring under ice-cooling, 2.20 g (55 mmol) of 60% sodium hydride (dispersion in oil). The mixture was stirred for 15 minutes at the same temperature. To the reaction mixture was added 14.10 g (50 mmol) of phthalimide, which was stirred for 6 hours at 100° C. After cooling, the reaction mixture was then poured into water, extracted with chloroform. The extract solution was dried over anhydrous magnesium sulfate, the solvent was distilled off. The residue was purified by column chromatography (eluent: ethyl acetate) to give 11.43 g of the desired compound (61.1%, pale yellow solid).

1. additionwas added
2. temperaturecooling
3. stirringThe mixture was stirred for 15 minutes at the same temperature
4. stirringwas stirred for 6 hours at 100° C
5. temperatureAfter cooling
6. extractionextracted with chloroform
7. dry with materialThe extract solution was dried over anhydrous magnesium sulfate
8. distillationthe solvent was distilled off
9. customThe residue was purified by column chromatography (eluent: ethyl acetate)