関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Resorcinol | HCID 5054 | — |
| 反応物 | 2-Chloro-4,6-diphenyl-1,3,5-triazine | HCID 19698 | — |
| 反応物 | Sodium Methoxide | HCID 10942334 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | O-Xylene | HCID 7237 | — |
| 溶媒 | Sulfolane | HCID 31347 | — |
| 生成物 | 2-(2,4-Dihydroxyphenyl)-4,6-diphenyl-1,3,5-triazine | HCID 135437125 | — |
反応手順
A 500 mL three-necked, round-bottomed flask equipped with a mechanical stirrer is charged with 60 g of xylene and 55.5 g (0.207) of 4,6-diphenyl-2-chloro-s-triazine. The mixture is warmed to 118° C. and the pressure is reduced to 300 mbar and 2.8 g of hydrogen chloride gas is charged to the system. The mixture is cooled to 80° C. and a solution of resorcinol (88.2 g, 0.802 mol) in 60 g of tetramethylene sulfone is added dropwise over a 7-minute period. The mixture is stirred at 80° C. for six hours and then for one hour at 100° C. The temperature is reduced to 60° C. and a 300 mL portion of methanol is added. The mixture is allowed to cool to room temperature and is stirred overnight. Sodium methoxide (41.3 g) is added portionwise to adjust the pH to 5.0-5.5. The solids are collected by vacuum filtration and are washed with methanol and water. After drying, the title compound is obtained in a yield of 59.2 g as a pale yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06242598B1 |
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| 出典データセット | uspto-grants-2001_06 |
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| ORD ID | ord-b4fb05a14f424cdcbcd193bd5795b8a8 |
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| 出典メモ | uspto-grants-2001_06 |
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