Ethanol → 2-Ethoxalyloxyethyl methacrylate

HRID 1197207

반응식

HRID 1197207 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].C1(C)C=CC(S(O)(=O)=O)=CC=1.C(C1C=C(O)C(C(C)(C)C)=CC=1O)(C)(C)C.C(O)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 5

HCID 702EthanolHCID 23742,5-Di-tert-butylhydroquinoneHCID 6101p-Toluenesulfonic acidHCID 7268Diethyl OxalateHCID 133602-Hydroxyethyl Methacrylate

생성물 1

HCID 194284412-Ethoxalyloxyethyl methacrylate수율 52.4%

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 2,5-di-t-butylhydroquinone (polymerization inhibitor) were added. The mixture was heated to keep about 130° C. for 3 hours in nitrogen atmosphere with distilling 23.5 ml (0.40 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 52.4% of 2-ethoxalyloxyethyl methacrylate (bp 95°-125° C./0.3 mmHg).

후처리

  1. customA 500 ml flask equipped with a decanter
  2. additionwere added
  3. temperatureThe mixture was heated
  4. customThe reaction mixture was evaporated
  5. customto remove excess diethyl oxalate
  6. distillationdistilled under vacuum

출처 및 근거

ORD 기록
ord-6a533ce4e8664dcfb4e421dc654d138b
출처 데이터셋
uspto-grants-1992_05
특허 번호
US05117044

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