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
- 80 °C
PROCEDURE
实验过程
A mixture of 3-acetylaminobenzylchloride (200 mg), 6-(4-hydroxy-3-(trifluoromethyl)-phenyl)-1-methyl-1H-imidazo[4,5-c]pyridine-4-carbonitrile (350 mg), sodium iodide (16 mg) and potassium carbonate (300 mg) in acetonitrile (20 ml) was heated at 80° C. for 14 hours. After cooling to room temperature, water (30 ml) was added, the white precipitate collected by filtration was dissolved in DMSO (1 ml) and purified by HPLC to give 6-(4-(3-acetylaminobenzoxy)-3-(trifluoromethyl)phenyl)-1H-imidazo[4,5-c]pyridine-4-carbonitrile. 1H NMR (DMSO) δ: 8.71 (s, 1H), 8.64 (s, 1H), 8.43 (m, 2H), 7.74 (s, 1H), 7.51 (m, 2H), 7.33 (t, 1H), 7.15 (d, 1H), 5.34 (s, 2H), 3.98 (s, 3H), 2.04 (s, 3H). MS m/z 466 (M+1).
WORKUP
后处理
- temperatureAfter cooling to room temperature
- filtrationthe white precipitate collected by filtration
- dissolutionwas dissolved in DMSO (1 ml)
- custompurified by HPLC