Oxalic Acid → Acrylic anhydride

HRID 1906706

반응식

HRID 1906706 반응식
[C:1]([OH:5])(=[O:4])[CH:2]=[CH2:3].C(O[C:10]([CH3:12])=[CH2:11])(C)=C.C(O)(=O)C(O)=[O:15]>C(Cl)Cl>[C:1]([O:5][C:12](=[O:15])[CH:10]=[CH2:11])(=[O:4])[CH:2]=[CH2:3]

참가 물질

5

반응물 3

HCID 971Oxalic AcidHCID 6581Acrylic AcidHCID 13483800Bisisopropenyl ether

생성물 1

HCID 74919Acrylic anhydride

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Acrylic acid (1.47 g, 0.02 mole), diisopropenyl ether (0.99 g, 0.01 mole) and oxalic acid (0.008 g, 8.9×10-5 moles) were mixed in a nitrogen-filled 10-ml volumetric flask. A 30-μl aliquot of this mixture was transferred to a nuclear magnetic resonance tube, mixed with CDCl3 (0.5 ml), methylene chloride (10 μ) and tetramethylsilane. After 24.5 hours, the sample in the nuclear magnetic resonance tube showed that the reaction was almost complete as the acid was nearly consumed. The amount of acrylic anhydride produced was 1.5:1 to that of the 2,2-propane diacrylate. Conversely the mixture in the original volumetric flask had a much lower conversion of reactants to products and almost no anhydride. After 14 days, the amount of acrylic anhydride in the nuclear magnetic resonance tube increased while that in the volumetric flask did not. The ratio of acrylic anhydride to 2,2-propane diacrylate was 3.3:1.

후처리

  1. additionfilled 10-ml volumetric flask
  2. customA 30-μl aliquot of this mixture was transferred to a nuclear magnetic resonance tube
  3. customwas nearly consumed

출처 및 근거

ORD 기록
ord-3368044ebe81404793d63d2bc170c085
출처 데이터셋
uspto-grants-1987_03
특허 번호
US04654174

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