反应 #1121720

反应方程式

triethylamine

4-methoxybenzoyl chloride

1,3-dimethyl-2-imidazolidinone

4-tert-butylacetophenone

→

uncolored oil

收率 7.0%

1-(4-Tert-butylphenyl)-vinyl 4-methoxybenzoate

收率 7.0%

溶剂

hexane ethyl acetate

chloroform

反应条件

后处理

1. 1
   其他The first collected fraction was purified twice by flash chromatography (hexane/dichloromethane 3:2 and next, hexane/dichloromethane 4:1)

实验过程

4-methoxybenzoyl chloride (2.35 g, 13.8 mmol), 0.65 g of cuprous chloride and 5.6 mL of 1,3-dimethyl-2-imidazolidinone were added to crude 4-tert-butylacetophenone trimethylsilylenol (6.7 mmol). After stirring the solution for 20 hours at room temperature, 1.4 mL of triethylamine and 10 mL of chloroform were added. Then the solution was chromatographied through flash silica column (hexane/ethyl acetate 10:1). The first collected fraction was purified twice by flash chromatography (hexane/dichloromethane 3:2 and next, hexane/dichloromethane 4:1) giving 0.14 g of an uncolored oil corresponding to 1-(4-tert-butylphenyl)-vinyl 4-methoxybenzoate. Yield 7%.

来源