HRID64087
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
A solution of N-(5-amino-2′,4′-difluorobiphenyl-3-yl)acetamide (3.0 g, 11.44 mmol), 4-bromo-1-fluoro-2-nitrobenzene (2.52 g, 11.44 mmol, 1.0 eq.) and potassium fluoride (0.663 g, 11.44 mmol, 1.0 eq.) in DMF was heated at 130° C. for 5 h. The mixture was quenched and extracted as in Example 1(d). The solvent was distilled off under reduced pressure and the crude residue was purified by column chromatography (60-120 silica gel, 40% ethyl acetate in hexane) to afford the product in 45% yield (2.4 g).
WORKUP
后处理
- customThe mixture was quenched
- extractionextracted as in Example 1(d)
- distillationThe solvent was distilled off under reduced pressure
- customthe crude residue was purified by column chromatography (60-120 silica gel, 40% ethyl acetate in hexane)
- customto afford the product in 45% yield (2.4 g)