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
CONDITIONS
反应条件
- 温度
- 85 °C
PROCEDURE
实验过程
To 5-[3-(2-chloro-4-pyrimidinyl)imidazo[1,2-a]pyridin-2-yl]-N-(2,6-difluorophenyl)-2-(methyloxy)benzamide (Intermediate Example 2) (0.12 g, 0.25 mmol) and 4-{5-[(dimethylamino)methyl]-1,3,4-oxadiazol-2-yl}-2-(methyloxy)aniline (0.069 g, 0.28 mmol) in trifluoroethanol (5 mL) was added HCl (0.050 mL, 4 M in dioxane, 0.20 mmol). The reaction was heated at 85° C. for 48 hours. Purification by flash chromatography followed by trituration with diethyl ether provided the title compound (0.089 g, 0.12 mmol, 51%). 1H NMR (400 MHz, DMSO-d6) δ ppm 2.23 (s, 6H), 3.76 (s, 2H), 3.96 (d, J=4.6 Hz, 6H), 6.76 (d, J=4.9 Hz, 1H), 7.03 (t, J=6.9 Hz, 1H), 7.15 (t, J=8.1 Hz, 2H), 7.26 (d, J=8.2 Hz, 1H), 7.30-7.40 (m, 1H), 7.42-7.50 (m, 1H), 7.51-7.59 (m, 2H), 7.71 (d, J=9.2 Hz, 1H), 7.78 (d, J=8.8 Hz, 1H), 8.10 (br. s., 1H), 8.35 (d, J=8.6 Hz, 1H), 8.39 (d, J=5.5 Hz, 1H), 8.69 (br. s., 1H), 9.44 (d, J=6.8 Hz, 1H), 9.74 (s, 1H). MS (M+H, ES+) 704.
WORKUP
后处理
- customPurification by flash chromatography