반응 #6500

ord-5bb43bb802e74697b19c498517a29caa

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 76.5%

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
    기타The reaction mixture was evaporated
  5. 5
    기타to remove excess diethyl oxalate
  6. 6
    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 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).

출처

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