참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Salicylaldehyde oxime | HCID 7200 | — |
| 반응물 | Cesium carbonate | HCID 10796 | — |
| 반응물 | 5-Bromo-2-chlorotoluene | HCID 609899 | — |
| 반응물 | HCID 178478050 | HCID 178478050 | — |
| 촉매 | Copper oxide | HCID 14829 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 1-(3-methyl-4-chlorophenyl)-3-(3-chlorophenyl)-1H-pyrazole | HCID 66787190 | 21.7% |
반응 단계
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).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08822521B2 |
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| 출처 데이터셋 | uspto-grants-2014_09 |
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| ORD ID | ord-eb7316c064804edc9d13bdbb0e2da187 |
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| 출처 메모 | uspto-grants-2014_09 |
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