Reaktion #6502

ord-1e1b570bc8ce444bb33a68c096a4880b

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeA 500 ml flask equipped with a decanter
  2. 2
    workup.ADDITIONwere added
  3. 3
    TemperaturThe mixture was heated
  4. 4
    Sonstigeat about 120° C.
  5. 5
    Sonstigefor 2 hours
  6. 6
    SonstigeThe reaction mixture was evaporated
  7. 7
    Sonstigeto remove excess diethyl oxalate
  8. 8
    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 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).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05248749uspto-grants-1993_09