HRID492990
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
4-[2-(Azetidin-1-yl)ethyl]piperazine-1-carboxylic acid [4-(2-fluoro-4-nitrophenoxy)pyridin-2-yl]amide (114 mg) was dissolved in tetrahydrofuran (3 ml) and methanol (3 ml). 10% Palladium carbon (55 mg) was added, followed by stirring under a hydrogen atmosphere for 22 hrs. The reaction mixture was filtered to remove the catalyst, and the catalyst was washed with methanol. The filtrate was concentrated under reduced pressure to give a residue, which was then purified by silica gel column chromatography (Fuji Silysia NH, eluent; ethyl acetate:methanol=9:1). Fractions containing the target compound were concentrated to give a crude product of the titled compound (71 mg) as a pale yellow oil.
WORKUP
后处理
- filtrationThe reaction mixture was filtered
- customto remove the catalyst
- washthe catalyst was washed with methanol
- concentrationThe filtrate was concentrated under reduced pressure
- customto give a residue, which
- customwas then purified by silica gel column chromatography (Fuji Silysia NH, eluent; ethyl acetate:methanol=9:1)
- additionFractions containing the target compound
- concentrationwere concentrated