HRID1363160
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 4-fluoro-3-nitrobenzonitrile (5.0 g) in THF (100 mL) was treated with DIEA (6.3 mL) and 2,4-dimethoxybenzylamine (5.0 mL), and then stirred for 24 h. The solvent was evaporated and the crude mixture was dissolved in EtOAc (100 mL). The solution was washed once with 1 M HCl and twice with saturated aqueous NaCl (100 mL each). The organic layer was separated, dried over Na2SO4, filtered, and concentrated in vacuo. Column chromatography (20% EtOAc/DCM) provided 9.25 g of the title compound.
WORKUP
后处理
- customThe solvent was evaporated
- dissolutionthe crude mixture was dissolved in EtOAc (100 mL)
- washThe solution was washed once with 1 M HCl and twice with saturated aqueous NaCl (100 mL each)
- customThe organic layer was separated
- dry with materialdried over Na2SO4
- filtrationfiltered
- concentrationconcentrated in vacuo