HRID1969021
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
[3-(4-Bromo-2-formyl-phenoxy)-phenyl]-acetic acid methyl ester (0.151 g, 0.43 mmol), benzylamine (0.05 mL, 0.48 mmol), and sodium cyanoborohydride (0.041 g, 0.65 mmol) were combined in CH2Cl2 (3 mL). Acetic acid (2 drops) was added, and the reaction was stirred overnight at room temperature. The mixture was partitioned between CH2Cl2 and saturated aqueous NaHCO3, and the aqueous layer was separated and extracted twice with CH2Cl2. The combined organic layers were dried over MgSO4 and concentrated, and the residue was purified by silica gel chromatography (10-30% EtOAc in hexanes) to give the title compound.
WORKUP
后处理
- customThe mixture was partitioned between CH2Cl2 and saturated aqueous NaHCO3
- customthe aqueous layer was separated
- extractionextracted twice with CH2Cl2
- dry with materialThe combined organic layers were dried over MgSO4
- concentrationconcentrated
- customthe residue was purified by silica gel chromatography (10-30% EtOAc in hexanes)