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Hydrochloric Acid → 2-(Fluoro-dichloro-methyl)-8-methyl-4-chloro-quinoline
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Antimony pentachloride | HCID 24294 | — |
| 反応物 | Antimony pentafluoride | HCID 24557 | — |
| 反応物 | 4-Chloro-8-methyl-2-(trichloromethyl)quinoline | HCID 15622255 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-(Fluoro-dichloro-methyl)-8-methyl-4-chloro-quinoline | HCID 15622256 | — |
反応手順
3.0 g of 2-trichloromethyl-8-methyl-4-chloro-quinoline are dissolved in 45 ml of dry dichloromethane and under intense stirring 1.5 ml of antimony-penta-chloride and 1.0 ml of antimony-penta-fluoride are added by dropping at a temperature of -5° to 0° C. The mixture is stirred at this temperature for 4 hours and allowed to stand at room temperature for 48 hours. 6 ml of icy concentrated hydrochloric acid are added, the precipitate is filtered, washed with some dichloromethane, the filtrate is separated, dried, filtered and evaporated. 2.1 g solid product are obtained which is recrystallized from heptane: 1.9 g of a yellowish crystalline substance, 68.2%, m.p.: 90°-94° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04659834 |
| 出典データセット | uspto-grants-1987_04 |
| ORD ID | ord-f9a3a7745e0a4edeb479b8851e6d1311 |
| 出典メモ | uspto-grants-1987_04 |