関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | 2,3-Dichloropyridine | HCID 16988 | — |
| 反応物 | HCID 178419412 | HCID 178419412 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-(3-Bromo-1H-pyrazol-1-yl)-3-chloropyridine | HCID 21071278 | 68.5% |
反応手順
A mixture of 10.7 g of 3-bromo-1H-pyrazole, 11.8 g of 2,3-dichloropyridine, 57.3 g of cesium carbonate and 80 ml of N,N-dimethylformamide was stirred at 100° C. for 8 hours. The reaction mixture was allowed to cool to room temperature. After water was added, and the reaction mixture was extracted with methyl tert-butyl ether two times. The organic layers were combined, washed with sequentially with water and a saturated solution of sodium chloride, dried over magnesium sulfate, and concentrated under reduced pressure. The resulting residue was subjected to silica gel column chromatography to obtain 12.9 g of 2-(3-bromo-1H-pyrazol-1-yl)-3-chloropyridine.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08541613B2 |
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| 出典データセット | uspto-grants-2013_09 |
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| ORD ID | ord-e4e8285435754c6d807f16ded550280b |
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| 出典メモ | uspto-grants-2013_09 |
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