関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1,1,1-Trichloro-2,2,2-trifluoroethane | HCID 9635 | — |
| 反応物 | Aluminum(III) Chloride | HCID 6451240 | — |
| 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 | HCID 23282361 | HCID 23282361 | 38% |
反応手順
Then, 19.54 g of 4-(2,6-dichloro-4-(3,3-dichloro-2-propenyloxy)phenoxy)butyloxyacetaldehyde was dissolved in 200 ml of N,N-dimethylformamide, to which 25.3 g of 1,1,1-trichlorotrifluoroethane, 17.6 g of zinc dust and 2.0 g of aluminum chloride were added. After stirring at room temperature for 1.5 hours, the reaction mixture was filtered. The filtrate was poured into diluted hydrochloric acid and extracted twice with diethyl ether. The diethyl ether layers were combined, washed with water, dried over magnesium sulfate and then concentrated to give a crude product. The crude product was subjected to silica gel chromatography, which afforded 8.46 g of 3,5-dichloro-1-(3,3-dichloro-2-propenyloxy)-4-(4-(3-chloro-4,4-difluoro-2-hydoxy-3-butenyloxy)butyloxy)benzene (yield, 38%), nD22.5 1.5302.
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-44e24706c43649f8978e8ee0a1e5db3f |
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| 出典メモ | uspto-grants-2000_10 |
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