참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Methyl 3-(dimethylamino)acrylate | HCID 566587 | — |
| 반응물 | 2,4-Dichloro-5-fluorobenzoyl chloride | HCID 2736821 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 생성물 | HCID 54215864 | HCID 54215864 | 89.1% |
반응 단계
First a solution of 12.9 g of methyl 3-dimethylaminoacrylate in 25 ml of dioxane is 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 3 hours, heated at 50°-60° C. for 1 hour, and the solvent is removed by distillation in vacuo and the residue is taken up in methylene chloride/H2O. 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. The crystalline residue is recrystallized from methanol/water. 28.5 g of methyl 3-dimethylamino-2-(2,4-dichloro-5-fluorobenzoyl)acrylate of melting point 107°-109° C. are obtained.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04699992 |
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| 출처 데이터셋 | uspto-grants-1987_10 |
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| ORD ID | ord-4f072d9b2f4943c599348ab0bb92c1e2 |
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| 출처 메모 | uspto-grants-1987_10 |
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