関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methacrylic Acid | HCID 4093 | — |
| 反応物 | Azobisisobutyronitrile | HCID 6547 | — |
| 反応物 | Poly(vinylphosphonic acid) | HCID 168725 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | Vinylphosphonic Acid Methacrylic Acid | HCID 86663293 | — |
反応手順
In a 10 liter flask equipped with a stirrer, a capacitor and a dropping device, 3,500 g of ethyl acetate was charged and heated to 70° C. Then, 390 g (3.61 mol) of a vinylphosphonic acid monomer, 1,243 g (14.44 mol) of methacrylic acid and 52 g of AIBN were dissolved in 1,000 g of ethyl acetate and the obtained solution was added dropwise in a reactor over 4 hours. During the dropwise addition of a monomer solution, a white precipitate was produced. After heating and stirring for 2 hours while maintaining at 70° C., heating was stopped and the reaction solution was cooled to room temperature. The precipitate thus produced was collected by filtration under reduced pressure and then washed with 1,000 g of ethyl acetate. The precipitate was vacuum-dried at 40° C. for 24 hours to obtain a white fine crystal. Yield: 1,550 g
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08835099B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-d412556cfedc4d898fb1b9e3ac99e0ab |
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| 出典メモ | uspto-grants-2014_09 |
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