HRID50944
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
Free base of the titled compound was prepared from 4-methoxy-2-amino-N-(2-pyridyl)aniline and (E)-4-methyl-2-pentenoyl chloride according to the preparation of (E)-1-(2-pyridyl)-2-styryl-1H-benzimidazole (Example 1, method A). The free base and oxalic acid were dissolved into ethyl acetate. Concentration and recrystallization from ethyl acetate/n-hexane yielded the titled compound. MW: 383.41; mp: 140.0-141.0° C.; 1H-NMR (DMSO) δ: 8.71 (1H, d, J=3.7 Hz), 8.16-8.10 (1H, m), 7.64-7.56 (2H, m), 7.28 (1H, d, J=9.2 Hz), 7.19 (1H, d, J=2.2 Hz), 6.99-6.83 (2H, m), 6.37 (1H, d, J=15.8 Hz), 3.80 (3H, s), 2.52-2.42 (1H, m), 1.02 (6H, d, J=6.6 Hz).
WORKUP
后处理
- concentrationConcentration and recrystallization from ethyl acetate/n-hexane