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HRID 1641466作成日:2026年10月25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/1641466
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-ethyl 3-bromo-1-(3-chloropyridin-2-yl)-1H-pyrazole-5-carbothioate | HCID 86639909 | — |
| 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 | 45.6% |
反応手順
0.35 g of S-ethyl 3-bromo-1-(3-chloropyridin-2-yl)-1H-pyrazole-5-carbothioate and 0.24 g of 2-amino-5-chloro-N-(1-cyclopropylethyl)benzamide were dissolved in 5 ml of dimethyl sulfoxide, and 0.85 g of anhydrous sodium sulfate was added, followed by stirring for 5 minutes. 0.14 g of potassium tert-butoxide was added at room temperature, followed by stirring for 1.5 hours. The reaction liquid was added to water, followed by extraction with ethyl acetate. The organic layer was washed with a saturated 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=1/0 to 1/1) to obtain 0.24 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-03f86ded675b4afea7a5b6b732205db2 |
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| 出典メモ | uspto-grants-2012_02 |
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