関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4-Chlorobiphenyl | HCID 16323 | — |
| 反応物 | Itaconic Anhydride | HCID 75110 | — |
| 反応物 | Aluminum(III) Chloride | HCID 6451240 | — |
| 溶媒 | Chlorobenzene | HCID 7964 | — |
| 生成物 | 2-[2-(4'-Chloro-biphenyl-4-YL)-2-oxo-ethyl]acrylic acid | HCID 9839318 | 75% |
反応手順
21.2 g of anhydrous aluminum chloride are introduced into 130 g of chlorobenzene and the mixture is cooled to 0° C. A solid mixture of 8.3 g of itaconic anhydride and 13.2 g of 4-chlorobiphenyl is added in portions in the course of one hour. The reaction mixture is stirred at 0° C. for three hours and then added to ice water. The solid reaction product is filtered off and washed twice with water (50 ml). The product is dried at room temperature and about 100 mbar until free of solvent and water. 4-(4′-Chlorobiphenyl-4-yl)-4-keto-2-methylenebutyric acid is obtained in a yield of 75% as a colorless, finely crystalline powder.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06265607B1 |
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| 出典データセット | uspto-grants-2001_07 |
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| ORD ID | ord-aea2525ceec34293be55e14484e9db21 |
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| 出典メモ | uspto-grants-2001_07 |
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