関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Oxalic Acid | HCID 971 | — |
| 反応物 | Acrylic Acid | HCID 6581 | — |
| 反応物 | Bisisopropenyl ether | HCID 13483800 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Acrylic anhydride | HCID 74919 | — |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04654174 |
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| 出典データセット | uspto-grants-1987_03 |
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| ORD ID | ord-3368044ebe81404793d63d2bc170c085 |
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| 出典メモ | uspto-grants-1987_03 |
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