HRID1006052
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
CONDITIONS
反应条件
- 温度
- 4 °C
PROCEDURE
实验过程
A mixture of 5-acenaphthylamine (1.0 g, 6 mmol) and triethylamine (0.76 g, 7.5 mmol) in toluene (50 mL) was stirred at 4° C., and 4-tert-butylbenzyl-bromide (1.36 g, 6 mmol) was added in slowly. The reaction mixture was stirred at 23° C. for 15 hours and precipitates formed. The precipitates (triethylamine.HBr) were filtered out; the filtrate was concentrated to dryness. Then the crude reaction mixture was purified by column chromatography (SiO2, hexane/CH2Cl2=5/1). N-(5-acenaphthyl)-4-tert-butylbenzylamine (1.67 g, an oil) was obtained.
WORKUP
后处理
- stirringThe reaction mixture was stirred at 23° C. for 15 hours
- customprecipitates
- customformed
- customThe precipitates (triethylamine.HBr)
- filtrationwere filtered out
- concentrationthe filtrate was concentrated to dryness
- customThen the crude reaction mixture
- customwas purified by column chromatography (SiO2, hexane/CH2Cl2=5/1)