関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Ethyl 3-(diethylamino)acrylate | HCID 139639 | — |
| 反応物 | 2,4-Dichloro-5-fluorobenzoyl chloride | HCID 2736821 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | Ethyl 3-diethylamino-2-(2,4-dichloro-5-fluorobenzoyl)acrylate | HCID 54148103 | 80.2% |
反応手順
First 17.1 g of ethyl 3-diethylaminoacrylate are added dropwise and then 10.5 g of triethylamine are added to a solution of 22.75 g of 2,4-dichloro-5-fluorobenzoyl chloride in 80 ml of anhydrous dioxane, while cooling in ice and stirring. The mixture is stirred at room temperature for one hour, heated to boiling under reflux for 45 minutes, and the solvent is removed by distillation in vacuo, and the oily residue is taken up in methylene chloride/water. The phases are separated, and the aqueous solution is again extracted with methylene chloride. The combined organic phases are washed with water, dried with sodium sulphate, and the methylene chloride is removed in vacuo. 29 g of ethyl 3-diethylamino-2-(2,4-dichloro-5-fluorobenzoyl)acrylate are obtained as a brown oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04699992 |
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| 出典データセット | uspto-grants-1987_10 |
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| ORD ID | ord-3d3b491826424629a8c5a2f225a8892a |
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| 出典メモ | uspto-grants-1987_10 |
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