反应 #6502
ord-1e1b570bc8ce444bb33a68c096a4880b
反应条件
详细条件
See reaction.notes.procedure_details.
后处理
- 1其他A 500 ml flask equipped with a decanter
- 2workup.ADDITIONwere added
- 3温度The mixture was heated
- 4其他at about 120° C.
- 5其他for 2 hours
- 6其他The reaction mixture was evaporated
- 7其他to remove excess diethyl oxalate
- 8workup.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 dibutyltin dilaurate (catalyst) and 4 g of 2,5-di-t-butylhydroquinone (polymerization inhibitor) were added. The mixture was heated to keep it at about 120° C. for 2 hours in nitrogen atmosphere with distilling 32.5 ml (0.56 mol) of ethanol away. The reaction mixture was evaporated to remove excess diethyl oxalate and then distilled under vacuum to obtain 84.2 g (yield 73.2%) of 2-ethoxalyloxyethyl methacrylate (bp 124° C./0.4 mmHg).