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HRID 1626758作成日:2026年10月27日

Sodium Iodide → HCID 66679973、化合物

https://huagongshe.com/reaction/1626758

反応式

関与物質

役割名称HCID仕込み量
反応物Sodium IodideHCID 5238—
反応物5-Chloro-2-((2-chloroacetyl)amino)benzoic acidHCID 4179825—
反応物4'-Fluoro-4-methylbiphenyl-3-amineHCID 46314430—
溶媒DimethylformamideHCID 6228—
溶媒Ethyl AcetateHCID 8857—
生成物HCID 66679973HCID 6667997320%

反応手順

1.0 g (4.0 mmol) of 5-chloro-2-[(chloroacetyl)amino]benzoic acid, 1.78 g (8.9 mmol) of 4′-fluoro-4-methylbiphenyl-3-amine, and 60 mg (0.4 mmol) of sodium iodide were stirred in 3 mL of DMF at 90° C. for 5.5 hours. Thereafter, the reaction mixture was diluted with ethyl acetate and washed with 1N hydrochloric acid. The organic layer was dried over anhydrous sodium sulfate and the solvent was distilled off under reduced pressure. The obtained crude product was separated and purified by silica gel column chromatography. The separated fractions containing a target compound were combined and condensed. Ethyl acetate was added to the residue, and solids were collected by filtration. The resulting solids were recrystallized using ethyl acetate/n-hexane, thereby giving 334 mg of the target 5-chloro-2-{[N-(4′-fluoro-4-methylbiphenyl-3-yl)glycyl]amino}benzoic acid (yield: 20%).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08785473B2
出典データセットuspto-grants-2014_07
ORD IDord-f18adea036704c36981cc7781230fb36
出典メモuspto-grants-2014_07