関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | Chloromethyl 4-fluorobenzoate | HCID 11401232 | — |
| 反応物 | HCID 178517507 | HCID 178517507 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | [3-(4-Trifluoromethylpyridin-2-yl)-1,2,4-oxadiazol-5-on-4-yl]methyl 4-fluorobenzoate | HCID 59570357 | 34.2% |
反応手順
Into 2 ml of N,N-dimethylformamide was suspended 0.07 g of sodium hydride (60% oily), and 0.3 g of 3-(4-trifluoromethylpyridin-2-yl)-1,2,4-oxadiazol-5-one was added at room temperature. After stirring for 15 minutes, 0.29 g of chloromethyl 4-fluorobenzoate was added, and the mixture was stirred at 70° C. for 4 hours. The reaction solution was allowed to cool to room temperature, and poured into an aqueous saturated ammonium chloride solution, followed by extraction with ethyl acetate three times. The organic layers were combined, washed with an aqueous saturated sodium chloride solution, dried with anhydrous magnesium sulfate, and concentrated. The residue was subjected to silica gel column chromatography to obtain 0.17 g of [3-(4-trifluoromethylpyridin-2-yl)-1,2,4-oxadiazol-5-on-4-yl]methyl 4-fluorobenzoate (present compound (38)).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08318776B2 |
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| 出典データセット | uspto-grants-2012_11 |
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| ORD ID | ord-2ae16a5139b847cba2266c2b81f198a7 |
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| 出典メモ | uspto-grants-2012_11 |
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