関与物質
| 役割 | 名称 | HCID | 仕込み量 |
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| 反応物 | Cyanuric chloride | HCID 7954 | — |
| 反応物 | n-Butyl-2,2,6,6-tetramethyl-4-piperidinamine | HCID 118285 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 2-Chloro-4,6-bis-(2,2,6,6-tetramethyl-4-piperidyl-butylamino)-1,3,5-triazine | HCID 11114220 | — |
反応手順
To a solution of 18.4 g of cyanuric chloride in 200 ml of dioxane was added dropwise, with stirring, a solution of 43.6 g of 4-butylamino-2,2,6,6-tetramethylpiperidine in 100 ml of dioxane at 20°-25° C. The mixture was stirred at the same temperature for 2 hours, after which it was stirred at 60°-70° C. for 2 hours. At the end of this time, the dioxane was distilled off and the residue was poured into a 10% aqueous solution of potassium carbonate and extracted with ethyl acetate. The extract was dried over anhydrous potassium carbonate, and then the ethyl acetate was distilled off. The resulting oil was purified by column chromatography through silica gel, eluted with a 20:1:1 by volume mixture of ethyl acetate, ethanol and triethylamine, to give the title compound in the form of crystals melting at 40°-42° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04533688 |
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| 出典データセット | uspto-grants-1985_08 |
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| ORD ID | ord-9da1fe9f6da34451a8adbe6533a12bd3 |
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| 出典メモ | uspto-grants-1985_08 |
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