関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Iodide | HCID 5238 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | TFMPP hydrochloride | HCID 3084246 | — |
| 反応物 | 4-(4-(2-Chloroethyl)phenyl)-2-methylthiazole hydrobromide | HCID 14726991 | — |
| 溶媒 | Methyl Isobutyl Ketone | HCID 7909 | — |
| 生成物 | 4-(4-(2-(4-(3-Trifluoromethylphenyl)piperazinyl)ethyl)phenyl)-2-methylthiazole | HCID 14727014 | — |
反応手順
To a 125 ml round-bottomed flask equipped with condenser and N2 inlet were added 2.39 g (7.5 mmol) of 4-(4-(2-chloroethyl)phenyl)-2-methylthiazole hydrobromide, 2.0 g (7.5 mmol) of N-(3-trifluoromethylphenyl)piperazine hydrochloride, 2.62 ml (15.0 mmol) of diisopropylethylamine, 1.59 g (15.0 mmol) of sodium carbonate, 5 mg of sodium iodide, and 50 ml of methylisobutylketone. The reaction was heated at reflux for 4.5 days, filtered hot to remove inorganic material, cooled, and the precipitate filtered and washed with ether and ethyl acetate. The solid was taken up in methylene chloride, hydrochloride gas bubbled through to precipitate the salt, and the resulting solid filtered, washed with methylene chloride, and dried to give a solid, m.p. 170°-175° C., 1.93 g (51%).
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-657c9b01e2664e808756328b3d3ef8e0 |
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| 出典メモ | uspto-grants-1990_01 |
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