反应 #6500

反应方程式

2-hydroxyethyl methacrylate

diethyl oxalate

ethanol

→

2-ethoxalyloxyethyl methacrylate

收率 76.5%

反应条件

后处理

1. 1
   其他A 500 ml flask equipped with a decanter
2. 2
   workup.ADDITIONwere added
3. 3
   温度The mixture was heated
4. 4
   其他The reaction mixture was evaporated
5. 5
   其他to remove excess diethyl oxalate
6. 6
   workup.DISTILLATIONdistilled under vacuum

实验过程

A 500 ml flask equipped with a decanter, a thermometer, a stirrer and an inlet for nitrogen gas was charged with 65.1 g (0.5 mol) of 2-hydroxyethyl methacrylate and 365.4 g (2.5 mol) of diethyl oxalate, to which 2 g (10 mmol) of p-toluenesulfonic acid (catalyst) and 4 g of 2-t-butylhydroquinone (polymerization inhibitor) were added. The mixture was heated to keep about 130° C. for 3 hours in nitrogen atmosphere with distilling 22 ml (0.38 mol) of ethanol away. The reaction mixture was evaporated to remove excess diethyl oxalate and then distilled under vacuum to obtain 64.8 g (yield 76.5%) of 2-ethoxalyloxyethyl methacrylate (bp 84°-125° C./0.4 mmHg).

来源