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HRID 369667作成日:2026年10月24日
1,1,1-Trichloro-2,2,2-trifluoroethane → 3,5-Dichloro-1-(3,3-dichloro-2-propenyloxy)-4-(4-(3,3-dichloro-4,4,4-trifluoro-2-hydroxybutyloxy)butyloxy)benzene
https://huagongshe.com/ja/reaction/369667
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
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| 反応物 | 1,1,1-Trichloro-2,2,2-trifluoroethane | HCID 9635 | — |
| 反応物 | 4-(2,6-Dichloro-4-(3,3-dichloro-2-propenyloxy)phenoxy)butyloxyacetaldehyde | HCID 53826908 | — |
| 触媒 | Zinc | HCID 23994 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 3,5-Dichloro-1-(3,3-dichloro-2-propenyloxy)-4-(4-(3,3-dichloro-4,4,4-trifluoro-2-hydroxybutyloxy)butyloxy)benzene | HCID 23282413 | 63.4% |
反応手順
To a mixture of 2.01 g of 4-(2,6-dichloro-4-(3,3-dichloro-2-propenyloxy)phenoxy)butyloxyacetaldehyde, 1.31 g of zinc dust and 10 ml of N,N-dimethylformamide was added 4.12 g of 1,1,1-trichlorotrifluoroethane. After stirring at room temperature for 1.5 hours, the reaction mixture was filtered. The filtrate was poured into 20 ml of diluted hydrochloric acid and extracted twice with 50 ml of ethyl acetate. The ethyl acetate layers were combined, washed with water, dried over magnesium sulfate and then evaporated to give a crude product. The crude product was subjected to silica gel chromatography, which afforded 1.76 g of 3,5-dichloro-1-(3,3-dichloro-2-propenyloxy)-4-(4-(3,3-dichloro-4,4,4-trifluoro-2-hydroxybutyloxy)butyloxy)benzene (yield, 63%), nD24.2 1.5188.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06140274 |
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| 出典データセット | uspto-grants-2000_10 |
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| ORD ID | ord-0618dde99335441b96a472b8e46bca52 |
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| 出典メモ | uspto-grants-2000_10 |
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