HRID554637
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 [5-(4-fluoro-2-formyl-phenyl)-pyridin-3-yl]-acetic acid ethyl ester (1.2 g, 4.18 mmol) in MeOH was added sodium cyanoborohydride (0.394 g, 6.26 mmol) and ethylamine (2M in THF; 3.13 mL, 6.26 mmol). Acetic acid (0.36 mL, 6.26 mmol) was added, and the reaction was stirred for 2 hours at room temperature. The mixture was concentrated, and the residue was dissolved in CH2Cl2 and washed with saturated aqueous NaHCO3 and H2O. The organic layer was dried over Na2SO4, filtered, and concentrated, and the residue was purified by silica gel chromatography (0-10% MeOH in CH2Cl2) to give [5-(2-ethylaminomethyl-4-fluoro-phenyl)-pyridin-3-yl]-acetic acid ethyl ester.
WORKUP
后处理
- concentrationThe mixture was concentrated
- dissolutionthe residue was dissolved in CH2Cl2
- washwashed with saturated aqueous NaHCO3 and H2O
- dry with materialThe organic layer was dried over Na2SO4
- filtrationfiltered
- concentrationconcentrated
- customthe residue was purified by silica gel chromatography (0-10% MeOH in CH2Cl2)