HRID1875176
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 a solution of 3-[(6-amino-2-fluoro-3-methylphenyl)oxy]-5-chlorobenzonitrile (7.422 g, 26.8 mmol) and ammonium acetate (0.207 g, 2.68 mmol) in acetonitrile (150 ml) was added NBS (5.01 g, 28.2 mmol) and the reaction mixture was stirred for two hours at rt. The solvent was removed and the crude material was purified via silica gel chromatography to give 3-[(2-amino-3-bromo-6-fluoro-5-methylphenyl)oxy]-5-chlorobenzonitrile (8.379 g, 23.56 mmol, 88% yield). 1H NMR (400 MHz, DMSO-d6) δ ppm 7.71 (s, 1H), 7.33 (s, 1H), 7.23-7.30 (m, 2H), 5.31 (s, 2H), 2.08 (s, 3 H).
WORKUP
后处理
- customThe solvent was removed
- customthe crude material was purified via silica gel chromatography