反应详情

A solution of 4-((5-(4-(bis(4-methoxybenzyl)amino)-6-methyl-1,3,5-triazin-2-yl)-6-(6-methoxypyridin-3-ylamino)pyridin-3-yl)(hydroxy)methyl)-N,N-dimethylbenzenesulfonamide (38.3 mg, 0.050 mmol) in TFA (1.0 mL) was heated at 100° C. in a sealed tube for 5 h. The dark solution was concentrated and purified by prep HPLC to give 4-((5-(4-amino-6-methyl-1,3,5-triazin-2-yl)-6-(6-methoxypyridin-3-ylamino)pyridin-3-yl)(hydroxy)methyl)-N,N-dimethylbenzenesulfonamide trifluoroacetate (25 mg, 0.039 mmol, 78% yield). The sample was recrystallized from dioxane and dried to give a yellow solid. 1H NMR (400 MHz, d6-DMSO) δ 11.79 (s, 1H); 10.37 (br. s., 1H); 9.20 (d, J=2.35 Hz, 1H); 8.60 (d, J=2.54 Hz, 1H); 8.49 (d, J=2.54 Hz, 1H); 8.12 (dd, J=8.80, 2.74 Hz, 1H); 7.85-8.00 (m, 3H); 7.78 (br. s., 1H); 7.56 (td, J=7.58, 1.27 Hz, 1H); 7.35-7.46 (m, 1H); 6.83 (d, J=8.80 Hz, 1H); 6.61 (d, J=9.39 Hz, 1H); 3.84 (s, 3H); 2.84 (d, J=4.50 Hz, 3H); 2.76 (d, J=4.69 Hz, 3H); 2.46 (s, 3H). 19F NMR (376 MHz, d6-DMSO) δ −74.57 (br. s., 3F). m/z (ESI, +ve ion) 523 (M+H)+.

1. concentrationThe dark solution was concentrated
2. custompurified by prep HPLC