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HRID 645301作成日:2026年10月26日
Ethyl Acetate → 4-(3-(3,5-Dichlorophenyl)-4,4,4-trifluoro-2-butenoyl)-N-(2-pyridylmethyl)benzoic acid amide
https://huagongshe.com/reaction/645301
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | 2-Pyridinemethanamine | HCID 19509 | — |
| 反応物 | 4-(3-(3,5-Dichlorophenyl)-4,4,4-trifluoro-2-butenoyl)benzoic acid | HCID 66735658 | — |
| 反応物 | 1-(3-(Diethylamino)propyl)-3-ethylcarbodiimide chloride | HCID 86626428 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 4-(3-(3,5-Dichlorophenyl)-4,4,4-trifluoro-2-butenoyl)-N-(2-pyridylmethyl)benzoic acid amide | HCID 66735361 | 27.6% |
反応手順
To a solution of 0.5 g of 4-(3-(3,5-dichlorophenyl)-4,4,4-trifluoro-2-butenoyl)benzoic acid that was synthesized under Synthetic Example 4 and 0.21 g of 2-picolylamine in 6 mL of N,N-dimethylformamide, 0.32 g of 1-(3-(diethylamino)propyl)-3-ethylcarbodiimide chloride was added at room temperature and the mixture was stirred for 72 hours. After the completion of reaction, 20 mL of ethyl acetate and 15 mL of saturated saline were added to the reaction solution, the mixture was separated to extract an aqueous layer with 10 mL of ethyl acetate whereto an organic layer was added, the resulting mixture was washed with 10 mL of water and dried with anhydrous sodium sulfate, and the solvent was distilled off under reduced pressure. After purification of the resulting residue using silica gel column chromatography that was eluted with ethyl acetate-hexane (5:1) to obtain 0.17 g of aimed product as resinous matter.
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-6fdbcdd4e796477d9300a9ac0b405854 |
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| 出典メモ | uspto-grants-2010_04 |
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