関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | M-Xylene | HCID 7929 | — |
| 反応物 | Cyanuric chloride | HCID 7954 | — |
| 反応物 | Aluminum(III) Chloride | HCID 6451240 | — |
| 溶媒 | Chlorobenzene | HCID 7964 | — |
| 生成物 | 1,3,5-Triazine, 2-chloro-4,6-bis(2,4-dimethylphenyl)- | HCID 71059 | — |
| 生成物 | 2,4,6-Tris(2,4-dimethylphenyl)-1,3,5-triazine | HCID 22475988 | — |
反応手順
To a stirring mixture of 1 eq of cyanuric chloride, 3.5 eq of AlCl3 in chlorobenzene, was added 0.036 eq of sulfuric acid as a 10% aq. solution at ice-bath temperature. After 10 min of stirring 1.9 eq of m-xylene was added. After 5 min at ice bath temperature the reaction mixture was allowed to warm to 10° C. After 1 h 20 min. HPLC analysis showed 89% of the cyanuric chloride had reacted to give 2-chloro-4,6-bis(2,4-dimethylphenyl)-1,3,5-triazine and 2,4,6-tris(2,4-dimethylphenyl)-1,3,5-triazine, which were present in a ratio of 89:11. HPLC analysis, after 3 h at 9-11° C., showed 94% of the cyanuric chloride had reacted to give 2-chloro-4,6-bis(2,4-dimethylphenyl)-1,3,5-triazine and 2,4,6-tris(2,4-dimethylphenyl)-1,3,5-triazine, which were present in a ratio of 95:5. HPLC analysis, after 5 h at 9-11° C. and 17 h at room temperature, showed 98.5% of the cyanuric chloride had reacted to give 2-chloro-4,6-bis(2,4-dimethylphenyl)-1,3,5-triazine and 2,4,6-tris(2,4-dimethylphenyl)-1,3,5-triazine, which were present in a ratio of 97:3.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06710177B2 |
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| 出典データセット | uspto-grants-2004_03 |
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| ORD ID | ord-dd34ed1325604f649e4c853212cec50c |
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| 出典メモ | uspto-grants-2004_03 |
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