HRID554605
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To 2-bromo-5-(trifluoromethyl)benzaldehyde (7.5 g, 29.6 mmol) in MeOH (80 mL) was added ethylamine (2M in MeOH; 30 mL, 60 mmol), sodium cyanoborohydride (3.7 g, 58.9 mmol), and acetic acid (1.7 mL, 26.2 mmol), and the reaction was stirred at room temperature for 4 days. The mixture was quenched with saturated aqueous NaHCO3 and extracted with CH2Cl2, and the combined organic layers were dried over MgSO4, filtered, and concentrated. The crude material was purified by silica gel chromatography (0-4% MeOH in CH2Cl2) to give (2-bromo-5-trifluoromethyl-benzyl)-ethyl-amine.
WORKUP
后处理
- customThe mixture was quenched with saturated aqueous NaHCO3
- extractionextracted with CH2Cl2
- dry with materialthe combined organic layers were dried over MgSO4
- filtrationfiltered
- concentrationconcentrated
- customThe crude material was purified by silica gel chromatography (0-4% MeOH in CH2Cl2)