Ethanol → 2-Ethoxalyloxyethyl methacrylate

HRID 6406

반응식

HRID 6406 반응식
[C:1]([O:6][CH2:7][CH2:8][OH:9])(=[O:5])[C:2]([CH3:4])=[CH2:3].[C:10](OCC)(=[O:16])[C:11]([O:13][CH2:14][CH3:15])=[O:12].C(O)C>C([O-])(=O)CCCCCCCCCCC.C([O-])(=O)CCCCCCCCCCC.C([Sn+2]CCCC)CCC.C(C1C=C(O)C(C(C)(C)C)=CC=1O)(C)(C)C>[C:1]([O:6][CH2:7][CH2:8][O:9][C:10]([C:11]([O:13][CH2:14][CH3:15])=[O:12])=[O:16])(=[O:5])[C:2]([CH3:4])=[CH2:3]

참가 물질

6

반응물 3

HCID 702EthanolHCID 7268Diethyl OxalateHCID 133602-Hydroxyethyl Methacrylate

생성물 1

HCID 194284412-Ethoxalyloxyethyl methacrylate수율 73.2%

시약·촉매·용매 2

HCID 23742,5-Di-tert-butylhydroquinone촉매HCID 9809426Di-n-butyldilauryltin촉매

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).

후처리

  1. customA 500 ml flask equipped with a decanter
  2. additionwere added
  3. temperatureThe mixture was heated
  4. customat about 120° C.
  5. customfor 2 hours
  6. customThe reaction mixture was evaporated
  7. customto remove excess diethyl oxalate
  8. distillationdistilled under vacuum

출처 및 근거

ORD 기록
ord-1e1b570bc8ce444bb33a68c096a4880b
출처 데이터셋
uspto-grants-1993_09
특허 번호
US05248749

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