反应详情

30 ml of a 1.0M solution of boron trichloride in methylene chloride was dropped into a solution of 2.00 g (5.41 mmol) of 4-(3,4-methylenedioxybenzyl)amino-6,7,8-trimethoxyquinazoline in 150 ml of chloroform under stirring at room temperature. The obtained mixture was stirred at room temperature for 2 days, followed by the addition of methanol and the obtained mixture was distilled under a reduced pressure to remove the solvent. This procedure was repeated thrice and the obtained residue was purified by silica gel column chromatography (chloroform/n-hexane). Hydrochloric acid/ethanol was added to the eluate and the obtained mixture was distilled under a reduced pressure to remove the solvent, followed by the addition of ethanol. The crystals thus formed were recovered by filtration. Thus, 0.59 g of the title compound was obtained as a colorless needle.

1. stirringThe obtained mixture was stirred at room temperature for 2 days
2. distillationthe obtained mixture was distilled under a reduced pressure
3. customto remove the solvent
4. customthe obtained residue was purified by silica gel column chromatography (chloroform/n-hexane)
5. additionHydrochloric acid/ethanol was added to the eluate
6. distillationthe obtained mixture was distilled under a reduced pressure
7. customto remove the solvent
8. additionfollowed by the addition of ethanol
9. customThe crystals thus formed
10. filtrationwere recovered by filtration