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HRID 1641464作成日:2026年10月27日
Sodium Sulfate → 3-bromo-N-(4-chloro-2-(1-cyclopropylethylcarbamoyl)phenyl)-1-(3-chloropyridin-2-yl)-1H-pyrazole-5-carboxamide
https://huagongshe.com/reaction/1641464
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Sulfate | HCID 24436 | — |
| 反応物 | Potassium tert-butoxide | HCID 23665647 | — |
| 反応物 | 2-amino-5-chloro-N-(1-cyclopropylethyl)benzamide | HCID 43533096 | — |
| 反応物 | S-benzyl 3-bromo-1-(3-chloropyridin-2-yl)-1H-pyrazole-5-carbothioate | HCID 86639908 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3-bromo-N-(4-chloro-2-(1-cyclopropylethylcarbamoyl)phenyl)-1-(3-chloropyridin-2-yl)-1H-pyrazole-5-carboxamide | HCID 66736193 | 41.9% |
反応手順
0.85 g of anhydrous sodium sulfate was added to a mixed solution comprising 0.24 g of 2-amino-5-chloro-N-(1-cyclopropylethyl)benzamide, 0.41 g of S-benzyl 3-bromo-1-(3-chloropyridin-2-yl)-1H-pyrazole-5-carbothioate and 5 ml of dimethyl sulfoxide at room temperature, followed by stirring for 5 minutes, and 0.14 g of potassium tert-butoxide was added, followed by reaction at room temperature for 1 hour. The reaction liquid was slowly added to water, the mixed liquid was subjected to extraction with ethyl acetate, and the organic layer was washed with a sodium chloride aqueous solution and dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure, and the residue was purified by silica gel column chromatography (eluent: n-hexane/ethyl acetate=9/1 to 7.5/2.5) to obtain 0.22 g of the desired product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08115006B2 |
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| 出典データセット | uspto-grants-2012_02 |
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| ORD ID | ord-36f05a2a6bec4b3fb2a0c9c96e1054e3 |
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| 出典メモ | uspto-grants-2012_02 |
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