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HRID 645302作成日:2026年10月26日
Water → N-(5-chloro-2-pyrimidinyl)-4-(3-(3,5-dichlorophenyl)-4,4,4-trifluoro-2-butenoyl)benzoic acid amide
https://huagongshe.com/reaction/645302
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
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| 反応物 | Water | HCID 962 | — |
| 反応物 | 2-Pyrimidinamine, 5-chloro- | HCID 79479 | — |
| 反応物 | 4-(3-(3,5-Dichlorophenyl)-4,4,4-trifluoro-2-butenoyl)benzoic acid chloride | HCID 87129944 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | N-(5-chloro-2-pyrimidinyl)-4-(3-(3,5-dichlorophenyl)-4,4,4-trifluoro-2-butenoyl)benzoic acid amide | HCID 86626430 | 50.5% |
反応手順
To a solution of 0.5 g of 2-amino-5-chloropyrimidine in 20 mL of pyridine, 0.5 g of 4-(3-(3,5-dichlorophenyl)-4,4,4-trifluoro-2-butenoyl)benzoic acid chloride was poured at room temperature and the mixture was stirred for 2.5 hours. After that, water was added to the reaction solution that was extracted with ethyl acetate, an organic layer was washed with water and diluted hydrochloric acid and then dehydrated and dried with saturated saline followed by anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. The resulting residue was purified using silica gel column chromatography that was eluted with ethyl acetate-hexane (5:2) followed by crystallization from a mixed solvent of hexane and a small amount of ethyl acetate to obtain 0.31 g of aimed product as white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07700808B2 |
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| 出典データセット | uspto-grants-2010_04 |
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| ORD ID | ord-936156af533845649de82c1a29311ee4 |
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| 出典メモ | uspto-grants-2010_04 |
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