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 20 minutes at the same temperature. To the reaction mixture was added 13.14 g (50 mmol) of N-(3-bromopropyl)phthalimide. The mixture was stirred for 7 hours at 100° C. After cooling, the reaction mixture was poured into water, which was subjected to extraction with chloroform. The extract was dried over anhydrous magnesium sulfate, and, the solvent was then distilled off. The residue was crystallized from methylene chloride--ethanol to give 5.72 g of the desired compound (31.7%, pale brown solid substance).

1. additionwas added
2. temperaturecooling
3. stirringThe mixture was stirred for 20 minutes at the same temperature
4. stirringThe mixture was stirred for 7 hours at 100° C
5. temperatureAfter cooling
6. extractionwas subjected to extraction with chloroform
7. dry with materialThe extract was dried over anhydrous magnesium sulfate
8. distillationthe solvent was then distilled off
9. customThe residue was crystallized from methylene chloride