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Oxalic Acid → Acrylic anhydride

HRID 1906706
ノート
印刷プレビュー

反応式

HRID 1906706 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 971Oxalic AcidHCID 6581Acrylic AcidHCID 13483800Bisisopropenyl ether

生成物 1

HCID 74919Acrylic anhydride

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-3368044ebe81404793d63d2bc170c085
出典データセット
uspto-grants-1987_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04654174

反応ノート

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