反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To the solution of 3-[8-(2,6-difluorophenyl)-2-(methylsulfinyl)-7-oxo-7,8-dihydropyrido[2,3-d]pyrimidin-4-yl]-4-methyl-N-1,3-thiazol-2-ylbenzamide (1.37 g, 2.54 mmol) in DCM (127 mL) were added Et3N (1.78 mL, 12.7 mmol) and (1H-imidazol-2-yl)-methylamine dihydrochloride (0.625 g, 3.81 mmol). The mixture was stirred at room temperature over night and concentrated under vacuum. Flash chromatography [mobile phase DCM/DCM (90)+MeOH(7)+NH4OH(3)] then provided the title compound as a white solid 1.23 g (85%). MS (ES) m/z 571 (M+H)+; 1H-NMR (MeOD) δ 2.16 (s, 1.5H), 2.32 (s, 1.5H), 3.18 (d, J=4.4 Hz, 0.75H), 4.11 (d, J=5.2 Hz, 0.25H), 4.21 (d, J=5.0 Hz, 1H), 4.50 (m, 1H), 6.37 (d, J=9.6 Hz, 1H), 6.85 (s, 2H), 7.29 (s, 2H), 7.43 (m, 2H), 7.57 (m, 3H), 8.18 (m, 3 H), 11.60 (s, br, 1H), 12.64 (s, br, 2H).
WORKUP
后处理
- concentrationconcentrated under vacuum