反应详情

To a solution of 1.22 g (5.0 mmol) of 1-[4-(amino) butan-1-yl]-1,2-dihydro-3-methyl-1,4,7b-triazacyclopent[cd]inden-2-one and 1.1 ml (7.9 mmol) of triethylamine in 40 ml of methylene chloride was added, while stirring under ice-cooling, 0.50 ml (6.5 mmol) of methyl chlorocarbonate. The mixture was stirred for 0.5 hour at room temperature. The reaction mixture was washed with an aqueous solution of sodium hydrogencarbonate, which was dried over anhydrous magnesium sulfate. The solvent was distilled off, and the residue was recrystallized from methylene chloride-methanol-ether to give 1.192 g of the desired compound (78.9%, colorless crystals), m.p.175-176° C.

1. temperaturecooling
2. stirringThe mixture was stirred for 0.5 hour at room temperature
3. washThe reaction mixture was washed with an aqueous solution of sodium hydrogencarbonate, which
4. dry with materialwas dried over anhydrous magnesium sulfate
5. distillationThe solvent was distilled off
6. customthe residue was recrystallized from methylene chloride-methanol-ether