HRID492676
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 1-(3-diethylaminopropyl)-3-[4-(2-fluoro-4-nitrophenoxy)pyridin-2-yl]urea (547 mg, 1.35 mmol) in methanol (40 ml)-tetrahydrofuran (20 ml) was added 10% palladium carbon (200 mg), followed by stirring under a hydrogen atmosphere at room temperature for 12 hrs. The catalyst was filtered and washed with methanol. The filtrate was concentrated under a reduced pressure to give a residue, which was then purified by silica gel column chromatography (Fuji Silysia NH, ethyl acetate, then ethyl acetate:methanol=10:1) to provide the titled compound (316 mg, 62.3%) as a yellow oil.
WORKUP
后处理
- filtrationThe catalyst was filtered
- washwashed with methanol
- concentrationThe filtrate was concentrated under a reduced pressure
- customto give a residue, which
- customwas then purified by silica gel column chromatography (Fuji Silysia NH, ethyl acetate