反应详情

A solution of 6-methoxy-7-(2-(N-methyl-N-(t-butylcarbonyl)amino)ethoxy)-3-((pivaloyloxy)methyl)-3,4-dihydroquinazolin-4-one (1.39 g, 3 mmol) in methylene chloride (4 ml) and TFA (4 ml) was stirred at ambient temperature for 1 hour. Toluene was added, and the volatiles were removed by evaporation. The residue was triturated with ether and the resulting solid was collected by filtration. The solid was dissolved in water, sodium hydrogen carbonate was added and the aqueous mixture was extracted with methylene chloride. The organic extract was dried (MgSO4) and the solvent removed by evaporation. The residue was triturated with ether and the solid was collected by filtration to give 6-methoxy-7-(2-(methylamino)ethoxy)-3-((pivaloyloxy)methyl)-3,4-dihydroquinazolin-4-one (800 mg, 73%). 1H NMR Spectrum: (DMSOd6; CF3COOD) 1.13(s, 9H); 2.72(s, 3H); 3.45(br s, 2H); 3.95(br s, 3H); 4.5(t, 2H); 5.94(s, 2H); 7.31(s, 1H); 7.6(s, 1H); 8.47(s, 1H) MS-ESI: 364 [MH]+

1. customthe volatiles were removed by evaporation
2. customThe residue was triturated with ether
3. filtrationthe resulting solid was collected by filtration
4. dissolutionThe solid was dissolved in water
5. additionsodium hydrogen carbonate was added
6. extractionthe aqueous mixture was extracted with methylene chloride
7. extractionThe organic extract
8. dry with materialwas dried (MgSO4)
9. customthe solvent removed by evaporation
10. customThe residue was triturated with ether
11. filtrationthe solid was collected by filtration