反应详情

To a solution of 2-[6-chloro-3-(2,2-difluoro-2-pyridin-2-yl-ethylamino)-2-oxo-2H-pyrazin-1-yl]-N-[2-(1-trityl-1H-imidazol-4-yl)-benzyl]-acetamide (47 mg, 0.058 mmol) in trifluoroacetic acid (1.5 ml) was added triethylsilane (excess) until completion of the reaction. Concentration and purification by reverse phase preparative HPLC (5% to 95% CH3CN in water containing 0.1% TFA, C18 PRO YMC 20×150 mm) gave 2-[6-chloro-3-(2,2-difluoro-2-pyridin-2-yl-ethylamino)-2-oxo-2H-pyrazin-1-yl]-N-[2-(1H-imidazol-4-yl)-benzyl]-acetamide TFA salt; 1H NMR (CD3OD, 400 MHz) δ 8.95 (d, 1H, J=1.3 Hz), 8.63 (d, 1H, J=4.1 Hz), 7.94 (dt, 1H, J=7.7 Hz, J=1.6 Hz), 7.70 (m, 2H), 7.51 (m, 6H), 6.83 (s, 1H), 4.80 (s, 2H), 4.46 (s, 2H), 4.28 (t, 2H, J=14.1 Hz); MS (ES+) M+1 500.4 for C23H20ClF2N7O2.

1. customuntil completion of the reaction
2. concentrationConcentration and purification by reverse phase preparative HPLC (5% to 95% CH3CN in water containing 0.1% TFA