تفاعل #6499

ord-f3ba761238a143e1b68d0ab2aac52f4d

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 hydroquinone (polymerization inhibitor) were added. The mixture was heated to keep 120° C. for 4 hours in nitrogen atmosphere with distilling 14 ml (0.25 mol) of ethanol away. The reaction mixture was evaporated to remove excess diethyl oxalate and then distilled under vacuum to obtain 88.1 g (yield 76.5%) of 2-ethoxalyloxyethyl methacrylate (colorless transparent liquid) (bp 98° C./0.3 mmHg).

المصدر

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