反应详情

Into a 8-dram vial, 4-(4-{7-[2-(Methanesulfonyl-methyl-amino)-phenyl]-pyrrolo[2,1-f][1,2,4]triazin-2-ylamino}-3-methoxy-benzyl)-piperazine-1-carboxylic acid tert-butyl ester (0.450 g, 0.724 mmol), Methylene chloride (15 mL, 230 mmol), and Trifluoroacetic Acid (3 mL, 40 mmol) were added. The reaction was stirred at room temperature overnight. The reaction was partitioned with saturated NaHCO3 and DCM. The organic was separated, washed with Brine and dried over Na2SO4. The solid was filtered and washed with DCM. The solvent was removed under vacuum to give N-{2-[2-(2-Methoxy-4-piperazin-1-ylmethyl-phenylamino)-pyrrolo[2,1-f][1,2,4]triazin-7-yl]-phenyl}-N-methyl-methanesulfonamide as an orange solid (0.37 g, 98%). LCMS (E/I+) 522.12 (M+H). NMR 1H (DMSO-d6)-8.95 (s, 1H), 7.95-7.99 (m, 1H), 7.87 (d, 1H, J=7.99 Hz), 7.72 (s, 1H), 7.60-7.67 (m, 1H), 7.50-7.57 (m, 2H), 7.07 (d, 1H, J=4.59 Hz), 6.96 (d, 1H, J=4.59 Hz), 6.93 (s, 1H), 6.72 (d, 1H, J=7.94 Hz), 3.83 (s, 3H), 3.37 (s, 3H), 3.04 (s, 3H), 2.88 (s, 3H), 2.73 (t, 4H, J=4.02 Hz), 2.29 (bs, 4H).

1. customThe reaction was partitioned with saturated NaHCO3 and DCM
2. customThe organic was separated
3. washwashed with Brine
4. dry with materialdried over Na2SO4
5. filtrationThe solid was filtered
6. washwashed with DCM
7. customThe solvent was removed under vacuum