반응 #6502

ord-1e1b570bc8ce444bb33a68c096a4880b

반응 방정식

C=C(C)C(=O)OCCO
2-hydroxyethyl methacrylate
CCOC(=O)C(=O)OCC
diethyl oxalate
CCO
ethanol
C=C(C)C(=O)OCCOC(=O)C(=O)OCC
2-ethoxalyloxyethyl methacrylate
수율 73.2%

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타A 500 ml flask equipped with a decanter
  2. 2
    workup.ADDITIONwere added
  3. 3
    온도The mixture was heated
  4. 4
    기타at about 120° C.
  5. 5
    기타for 2 hours
  6. 6
    기타The reaction mixture was evaporated
  7. 7
    기타to remove excess diethyl oxalate
  8. 8
    workup.DISTILLATIONdistilled under vacuum

실험 절차

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).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05248749uspto-grants-1993_09