참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 4-Chlorobenzenebromide | HCID 86664079 | — |
| 반응물 | HCID 178469268 | HCID 178469268 | — |
| 촉매 | Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI) | HCID 24350 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | Ethyl 1-(4-chlorophenyl)pyrazole-3-carboxylate | HCID 14129378 | 50% |
반응 단계
A 50 mL of flask was charged with 2.87 g of 4-chlorobenzenebromide (15 mmol), 1.40 g of ethyl 1-H-pyrazole-3-carboxylate (10 mmol), 400 mg of CuI (2.0 mmol), 4.5 g of K2CO3 (3.3 mmol) and 0.9 mL of trans-N,N′-dimethylcyclohexayldiamine (2.0 mmol). The resulting mixture was stirred at 140° C. for 3 h. After the mixture was cooled down to room temperature, it was diluted with 200 mL EtOAc and then was washed with water (2×50 mL) and brine (2×50 mL). The organics were dried over MgSO4 and concentrated under reduced pressure. The residued was purified via flash column chromatography on silica gel (0-25% EtOAc in hexanes) to get the desired product (1.25 g, 50%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09169261B2 |
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| 출처 데이터셋 | uspto-grants-2015_10 |
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| ORD ID | ord-905f48c402f64c8b98b6d28604c9e167 |
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| 출처 메모 | uspto-grants-2015_10 |
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