Reaktion #6500

Reaktionsgleichung

2-hydroxyethyl methacrylate

diethyl oxalate

ethanol

→

2-ethoxalyloxyethyl methacrylate

Ausbeute 76.5%

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeA 500 ml flask equipped with a decanter
2. 2
   workup.ADDITIONwere added
3. 3
   TemperaturThe mixture was heated
4. 4
   SonstigeThe reaction mixture was evaporated
5. 5
   Sonstigeto remove excess diethyl oxalate
6. 6
   workup.DISTILLATIONdistilled under vacuum

Vorschrift

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).

Quelle