関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 1-(1-Naphthyl)piperazine | HCID 1342 | — |
| 反応物 | Sodium Iodide | HCID 5238 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | 4-(2-Chloroethyl)phenyl-2-aminothiazole hydrobromide | HCID 14726983 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 溶媒 | Ethylacetate methanol | HCID 21584119 | — |
| 生成物 | 4-(4-(2-(4-(1-Naphthyl)piperazinyl)ethyl)phenyl)-2-aminothiazole | HCID 14726992 | — |
反応手順
To a 35 ml round-bottomed flask equipped with condenser and N2 inlet were added 3.19 g (10 mmol) of 4-(4-(2-chloroethyl)phenyl)-2-aminothiazole hydrobromide, 2.12 g (10 mmol) of N-(1-naphthyl)piperazine, 2.79 ml (20 mmol) of triethylamine, 1.06 g (10 mmol) of sodium carbonate, 2 mg of sodium iodide, and 25 ml of ethanol. The reaction was heated at reflux for 5 days, cooled, and the precipitate filtered, and washed with ethanol and water. The orange solid was chromatographed on silica gel using ethyl acetate/methylene chloride as eluent to give a white solid. The solid was taken up in ethyl acetate/methanol, ether saturated with HCl added, the precipitate filtered, washed with ether, and dried to give a white solid, 1.61 g (31%), m.p. 274°-277° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04891375 |
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| 出典データセット | uspto-grants-1990_01 |
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| ORD ID | ord-6a3a57f9eff3466ca564a9e901b59cec |
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| 出典メモ | uspto-grants-1990_01 |
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