関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 5-Bromo-2-furanecarboxylic acid | HCID 68511 | — |
| 反応物 | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| 反応物 | 3-[2,6-Dichloro-4-(3,3-dichloro-allyloxy)-phenoxy]-propylamine | HCID 15869744 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 3,5-Dichloro-1-(3,3-dichloro-2-propenyloxy)-4-(3-(5-bromo-2-furancarboxamido)propyloxy)-benzene | HCID 22006771 | 67.9% |
反応手順
To a mixture of 0.35 g of 4-(3-aminopropyloxy)-3,5-dichloro-1-(3,3-dichloro-2-propenyloxy)benzene, 0.19 g of 5-bromo-2-furancarboxylic acid, 0.18 ml of triethylamine and 10 ml of chloroform was added 0.23 g of WSC hydrochloride, while stirring at room temperature. After stirring at room temperature for 6 hours, the reaction mixture was concentrated to give a residue. The residue was dissolved in 50 ml of ethyl acetate, and the ethyl acetate layer was successively washed with 10% hydrochloric acid, saturated aqueous sodium hydrogen carbonate solution and saturated saline solution, dried over anhydrous magnesium sulfate, and then concentrated to give a residue. The residue was subjected to silica gel chromatography, which afforded 0.35 g of 3,5-dichloro-1-(3,3-dichloro-2-propenyloxy)-4-(3-(5-bromo-2 -furancarboxamido)propyloxy)benzene (64% yield), nD24.0 1.5918.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06028100 |
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| 出典データセット | uspto-grants-2000_02 |
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| ORD ID | ord-90fd8e9d3e7d48c5bc03484c0e6da5bf |
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| 出典メモ | uspto-grants-2000_02 |
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