反应详情

To a solution containing [1-(4-Chloro-2-methylbenzyl)-2-oxo-2-(4-quinazolin-4-yl-piperazin-1-yl)-ethyl]-carbamic acid tert-butyl ester (0.30 g, 0.59 mmol) in 30 mL of DCM under a nitrogen atmosphere was added TFA (1.4 mL.) After stirring at room temperature overnight, the reaction was concentrated under reduced pressure. The residue was dissolved in DCM and 2N HCl in ether added. The solids were filtered and dried to afford 2-Amino-3-(4-chloro-2-methyl-phenyl)-1-(4-quinazolin-4-yl-piperazin-1-yl)-propan-1-one dihydrochloride (0.217 g) as an off-white solid. LCMS (APCI+) m/z 410 [M+H]+; Rt: 1.87 min. 1H NMR (D2O, 400 MHz) δ 8.48 (1H, s), 7.91-7.86 (2H, m), 7.66-7.59 (2H, m), 7.08-7.02 (2H, m), 4.60-4.54 (1H,m), 4.20-4.12 (1H, m), 3.86-3.72 (3H, m), 3.61-3.38 (2H, m), 3.28-3.16 (2H, m), 3.01-2.94 (1H, m), 2.76-2.68 (1H, m), 2.19 (3H, s.)

1. concentrationthe reaction was concentrated under reduced pressure
2. dissolutionThe residue was dissolved in DCM
3. addition2N HCl in ether added
4. filtrationThe solids were filtered
5. customdried