関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Cyanuric chloride | HCID 7954 | — |
| 反応物 | 3-Hexen-1-ol | HCID 10993 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2,4,6-Tri(3-hexene-1-oxy)-1,3,5-triazine | HCID 89610595 | 61% |
反応手順
To 16.6 g of sodium hydride (purity: 60% or more), 600 mL of tetrahydrofuran was added and the resultant reaction mixture was cooled down to 0° C., followed by dropping 40.1 g of 3-hexen-1-ol into the reaction mixture at 4° C. or less to be added. After the completion of the dropping, the resultant reaction mixture was stirred at room temperature for 3 hours. Then, the reaction mixture was cooled down again to 0° C. and into the reaction mixture, 18.4 g of 2,4,6-trichloro-1,3,5-triazine dissolved in 120 mL of tetrahydrofuran was slowly dropped at 15° C. or less to be added. At room temperature, the reaction was effected over one night and to the reaction mixture, water was added, followed by extracting the resultant reaction mixture with ethyl acetate. The extract was washed with water and was dried over anhydrous sodium sulfate and from the extract, the solvent was distilled off to obtain 33.1 g of a crude product. The crude product was purified with a column (ethyl acetate:hexane=1:10) to obtain 23.22 g of 2,4,6-tri(3-hexene-1-oxy)-1,3,5-triazine which is the objective substance as a transparent oil. Yield: 61%, Purity: 98.6% (GC)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09102663B2 |
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| 出典データセット | uspto-grants-2015_08 |
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| ORD ID | ord-757c3581be944a5bb2db3c7136290285 |
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| 出典メモ | uspto-grants-2015_08 |
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