反应详情

Synthesized from compound 24. To a solution of 24 (1.5 g, 3.7 mmol) in 30 mL of CH2Cl2 was added 6 mL of TFA while stirring at room temperature. After 30 minutes, the solvents were evaporated and the residue was washed with acetonitrile to afford 1.0 g (90%) of analytically pure white solid. MP: 147-149° C.; MS (ES−): 297; 1H NMR (400 MHz, D2O): 1.96 (m, 2H), 2.82 (t, 2H), 3.01 (t, 2H), 3.28 (t, 4H), 3.53 (s, 2H), 7.22 (d, 1H), 7.47 (d, 1H), 7.61 (t, 1H). Anal. Calcd. for C15H18N6O. 1.1 CF3CO2H. 1.0H2O: C, 46.76; H, 4.81; N, 19.02. Found: C, 46.64; H, 4.98; N, 19.02.

1. customthe solvents were evaporated
2. washthe residue was washed with acetonitrile
3. customto afford 1.0 g (90%) of analytically pure white solid