反应详情

1.00 g (3.7 mmol) of ethyl 8-amino-1-methyl-1H-pyrazolo[4,3-h]quinazoline-3-carboxylate were dissolved in 50 mL of pyridine and 1 mL (8.0 mmol) of trichloroacetylisocyanate were added. The mixture was stirred overnight at room temperature. The solvent was then evaporated under reduced pressure and the residue was treated with 50 mL of methanol. After 2 hours under stirring the solvent was removed, the residue redissolved with dichloromethane and washed with a diluted solution of ammonium hydrate. After drying over anhydrous Na2SO4 the organic layer was evaporated to dryness and the residue purified by chromatography on a silica gel column (eluant: dichloromethane/acetone 4/1) leading 0.40 g (34% yield) of the title compound.

1. customThe solvent was then evaporated under reduced pressure
2. additionthe residue was treated with 50 mL of methanol
3. stirringAfter 2 hours under stirring the solvent
4. customwas removed
5. dissolutionthe residue redissolved with dichloromethane
6. washwashed with a diluted solution of ammonium hydrate
7. dry with materialAfter drying over anhydrous Na2SO4 the organic layer
8. customwas evaporated to dryness
9. customthe residue purified by chromatography on a silica gel column (eluant: dichloromethane/acetone 4/1)