反应详情

温度

50 °C

4 ml of dimethyl sulfoxide and 260 mg of methyl isocyanate were added to 500 mg of 2-amino-4-(3,4-methylenedioxybenzyl)amino-6-chloroquinazoline. The obtained mixture was stirred at 50° C. for 3 hours and distilled under a reduced pressure to remove excess methyl isocyanate, followed by the addition of chloroform and water. The mixture thus obtained was filtered and the filtrate was extracted with chloroform twice. The organic layers were combined, washed with water twice, dried over magnesium sulfate and distilled under a reduced pressure to remove the solvent. The residue was purified by silica gel column chromatography (benzene/acetone) and recrystallized (from benzene/chloroform/ethanol) to give 72 mg of the title compound.

1. distillationdistilled under a reduced pressure
2. customto remove excess methyl isocyanate
3. additionfollowed by the addition of chloroform and water
4. customThe mixture thus obtained
5. filtrationwas filtered
6. extractionthe filtrate was extracted with chloroform twice
7. washwashed with water twice
8. dry with materialdried over magnesium sulfate
9. distillationdistilled under a reduced pressure
10. customto remove the solvent
11. customThe residue was purified by silica gel column chromatography (benzene/acetone)
12. customrecrystallized (from benzene/chloroform/ethanol)