関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Salicylaldehyde oxime | HCID 7200 | — |
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | 5-Bromo-2-chlorotoluene | HCID 609899 | — |
| 反応物 | HCID 178478050 | HCID 178478050 | — |
| 触媒 | Copper oxide | HCID 14829 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1-(3-methyl-4-chlorophenyl)-3-(3-chlorophenyl)-1H-pyrazole | HCID 66787190 | 21.7% |
反応手順
A mixture of 3-(3-chlorophenyl)-1H-pyrazole (5.3 g, 29.8 mmol) (prepared according to the method given in European Patent Publication EP 538156), salicylaldoxime (0.58 g, 4.25 mmol), 5-bromo-2-chlorotoluene (2.8 g, 21.3 mmol), copper oxide (0.15 g, 1.06 mmol) and cesium carbonate (11.8 g, 36.2 mmol) in 20 mL of N,N-dimethylformamide was heated at 140° C. overnight and then allowed to cool to room temperature. The resulting suspension was filtered and the filtrate was concentrated under reduce pressure. The resulting residue was purified by medium pressure liquid chromatography (2 to 10% gradient of ethyl acetate in hexanes as eluant) to give the title compound as a white solid (1.4 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08822521B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-eb7316c064804edc9d13bdbb0e2da187 |
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| 出典メモ | uspto-grants-2014_09 |
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