تفاعل #6500

ord-5bb43bb802e74697b19c498517a29caa

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىA 500 ml flask equipped with a decanter
  2. 2
    workup.ADDITIONwere added
  3. 3
    درجة الحرارةThe mixture was heated
  4. 4
    أخرىThe reaction mixture was evaporated
  5. 5
    أخرىto remove excess diethyl oxalate
  6. 6
    workup.DISTILLATIONdistilled under vacuum

الإجراء التجريبي

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).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05248749uspto-grants-1993_09