関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Phosphoric Acid | HCID 1004 | — |
| 反応物 | Maleic Anhydride | HCID 7923 | — |
| 反応物 | 4-Methoxyphenol | HCID 9015 | — |
| 反応物 | Dodecylamine | HCID 13583 | — |
| 触媒 | Zinc Acetate | HCID 11192 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | O-Xylene | HCID 7237 | — |
| 生成物 | 1H-Pyrrole-2,5-dione, 1-dodecyl- | HCID 87191 | — |
反応手順
A glass flask having an inner volume of 3 liters was fitted with a theremometer, a stirrer and a water separater. This reactor was charged with 240 g of a xylene solution containing 120 g of maleic anhydride. Then, a solution of 220 g of dodecylamine in 1880 g of xylene was added thereto gradually and piecemeal at 40° C. over a period of 120 minutes. After the addition was completed, the resultant mixture and 65.4 g of ortho-phosphoric acid (purity 89% by weight), 0.672 g of p-methoxyphenol, and 0.05 g of zinc acetate added thereto were heated at 150° C. for four hours to effect reaction. Thereafter, the resultant reaction mixture was cooled to 30° C., washed with 400 ml of water, and separated into a water layer and a xylene layer. The xylene layer was filtered to effect removal of insolubles. The xylene layer now free from insolubles was distilled to expel xylene. Consequently there was obtained 260 g of slightly impure N-dodecyl maleimide. It was found to have purity of 91.2% by weight, indicating the yield thereof to be 75.3 mol % based on dodecylamine.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04780546 |
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| 出典データセット | uspto-grants-1988_10 |
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| ORD ID | ord-845715f9f7284fbf9c7e7e7f06ca61af |
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| 出典メモ | uspto-grants-1988_10 |
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