HRID220023
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
14 g (45 mmol) of methyl 5-[4-(trifluoromethoxy)phenyl]pyridine-3-carboxylate in ethanol (500 ml) were admixed with 17 g of moistened palladium/carbon catalyst (10% palladium, 50% water), and then hydrogenated at 60° C. and a 50 bar hydrogen atmosphere overnight. The reaction solution was filtered, the filter residue was washed with ethanol and the filtrate was concentrated under reduced pressure. The residue was purified by means of column chromatography (silica gel, dichloromethane/methanol 600:1→10:1). Yield: 8 g (59% of theory)
WORKUP
后处理
- customhydrogenated at 60° C.
- filtrationThe reaction solution was filtered
- washthe filter residue was washed with ethanol
- concentrationthe filtrate was concentrated under reduced pressure
- customThe residue was purified by means of column chromatography (silica gel, dichloromethane/methanol 600:1→10:1)