関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1-(4-Methoxyphenyl)-piperazine, dihydrochloride | HCID 2723700 | — |
| 反応物 | 3-(3-Chloropropyl)-6-fluorobenzo[d]isoxazole | HCID 10910880 | — |
| 触媒 | Potassium Iodide | HCID 4875 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1-[3-(6-Fluoro-1,2-benzisoxazol-3-yl)propyl]-4-(4-methoxyphenyl)piperazine oxalate | HCID 13520743 | 86.6% |
反応手順
To 40 ml of dimethylformamide was added 4.3 g 3-(3-chloropropyl)-6-fluoro-1,2-benzisoxazole, 4.0 g of 4-(4-methoxyphenyl)piperazine dihydrochloride, 10.0 g of milled potassium carbonate, and 0.01 g potassium iodide. The mixture was stirred at 90° C. for two hrs, cooled, filtered, and the filtrate evaporated to an oil. The oil was stirred with 100 ml of water and extracted with ether. The ether extract was washed with water (2×), saturated sodium chloride solution and dried over anhydrous magnesium sulfate. After filtering, ethereal oxalic acid was added. The precipitate was collected and dried to yield 3.0 g (44%) of product. Two recrystallizations from ethyl acetate/methanol/ether (10:1:5) gave the analytical sample, mp 188°-189° C. (dec).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04610988 |
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| 出典データセット | uspto-grants-1986_09 |
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| ORD ID | ord-f2823daaa5024119926dc8de134239a6 |
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| 出典メモ | uspto-grants-1986_09 |
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