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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

反応式

関与物質

役割名称HCID仕込み量
反応物Ethyl AcetateHCID 8857—
反応物2-PyridinemethanamineHCID 19509—
反応物4-(3-(3,5-Dichlorophenyl)-4,4,4-trifluoro-2-butenoyl)benzoic acidHCID 66735658—
反応物1-(3-(Diethylamino)propyl)-3-ethylcarbodiimide chlorideHCID 86626428—
溶媒DimethylformamideHCID 6228—
生成物4-(3-(3,5-Dichlorophenyl)-4,4,4-trifluoro-2-butenoyl)-N-(2-pyridylmethyl)benzoic acid amideHCID 6673536127.6%

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

DOI10.6084/m9.figshare.5104873.v1
特許番号US07700808B2
出典データセットuspto-grants-2010_04
ORD IDord-6fdbcdd4e796477d9300a9ac0b405854
出典メモuspto-grants-2010_04