関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Cyanuric chloride | HCID 7954 | — |
| 反応物 | (4-Bromophenylethynyl)trimethylsilane | HCID 4226980 | — |
| 反応物 | Magnesium | HCID 5462224 | — |
| 反応物 | HCID 178418255 | HCID 178418255 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2,4-Bis(4-ethynylphenyl)-6-phenyl-1,3,5-triazine | HCID 20429680 | — |
反応手順
One mole of cyanuric chloride was treated with one mole of phenylmagnesium bromide as described in Step I of Example I. The product of this reaction (2.3 g, 0.01 mole) in 25 ml of tetrahydrofuran (THF) was added slowly to a refluxing solution of the Grignard reagent prepared from 1-(trimethylsilyl)-2-(4-bromophenyl)acetylene (0.03 moles) and magnesium (0.75 g). The solution was stirred overnight, filtered, and the solvent removed. To the residue which remained was added a solution of KOH (10.0 g) in water (5 ml), anhydrous ethanol (100 ml) and dioxane (100 ml). The resulting mixture was heated for 2.5 hours at 60° C., filtered, and the solvent removed. Chromatographic separation of the resulting residue yielded a yellow solid, 6-phenyl-2,4-bis(4-ethynylphenyl)-s-triazine, which melted at approximately 215° C. with rapid polymerization.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04442278 |
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| 出典データセット | uspto-grants-1984_04 |
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| ORD ID | ord-4bf43c85562b43df8b7424e0a6d50c11 |
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| 出典メモ | uspto-grants-1984_04 |
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