反応 #6501

反応方程式

2-hydroxyethyl methacrylate

diethyl oxalate

ethanol

→

2-ethoxalyloxyethyl methacrylate

収率 56.3%

反応条件

後処理

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

実験手順

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 2,5-di-t-butylhydroquinone (polymerization inhibitor) were added. The mixture was heated to keep about 130° C. for 3 hours in nitrogen atmosphere with distilling 23.5 ml (0.40 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 52.4%) of 2-ethoxalyloxyethyl methacrylate (bp 95°-125° C./0.3 mmHg).

出典