関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Iodide | HCID 5238 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | TFMPP hydrochloride | HCID 3084246 | — |
| 反応物 | 4-(2-Chloroethyl)phenyl-2-aminothiazole hydrobromide | HCID 14726983 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 4-(4-(2-(4-(3-Trifluoromethylphenyl)piperazinyl)ethyl)phenyl)-2-aminothiazole | HCID 14211436 | — |
反応手順
To a 35 ml round-bottomed flask equipped with condenser and N2 inlet were added 0.81 g (2.55 mmol) of 4-(4-(2-chloroethyl)phenyl)-2-aminothiazole hydrobromide, 0.68 g (2.55 mmol) of N-(3-trifluoromethylphenyl)piperazine hydrochloride, 1.06 ml (7.64 mmol) of triethylamine, 0.27 g (2.55 mmol) of sodium carbonate, 2 mg of sodium iodide, and 10 ml of ethanol. The reaction was heated at reflux for 8 days, cooled, and the precipitate filtered, and the reaction mixture taken up in ethyl acetate/water. The layers were separated, the ethyl acetate washed with brine, dried, and evaporated to give a white solid, which was triturated with ethyl acetate. 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, 0.255 g (18%), 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-97602c7bc3e047e2802381429e7e193b |
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| 出典メモ | uspto-grants-1990_01 |
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