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Hydrochloric Acid → 3,5-Dichloro-1-(3,3-dichloro-2-propenyloxy)-4-(4-(3-chloro-3-ethoxycarbonyl-2-propenyloxy)butyloxy)benzene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Ethyl trichloroacetate | HCID 10588 | — |
| 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-chloro-3-ethoxycarbonyl-2-propenyloxy)butyloxy)benzene | HCID 53832795 | 5% |
反応手順
To a mixture of 0.60 g of 4-(2,6-dichloro-4-(3,3-dichloro-2-propenyloxy)phenoxy)butyloxyacetaldehyde, 0.29 g of zinc dust and 10 ml of N,N-dimethylformamide was added ethyl trichloroacetate with stirring at room temperature. After stirring at room temperature for 2 hours, the reaction mixture was poured into 10 ml of diluted hydrochloric acid and extracted twice with diethyl ether. The diethyl ether 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 0.04 g of 3,5-dichloro-1-(3,3-dichloro-2-propenyloxy)-4-(4-(3-chloro-3-ethoxycarbonyl-2-propenyloxy)butyloxy)benzene (yield, 5%), nD23.0 1.5348.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06140274 |
| 出典データセット | uspto-grants-2000_10 |
| ORD ID | ord-5d15c627687f44229f5bee816b68686d |
| 出典メモ | uspto-grants-2000_10 |