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HRID 131282作成日:2026年10月26日

Potassium Carbonate → 4-[2-(Dimethylamino)ethylthio]-benzoic acid

https://huagongshe.com/reaction/131282

反応式

関与物質

役割名称HCID仕込み量
反応物Potassium CarbonateHCID 11430—
反応物Captamine HydrochlorideHCID 25798—
反応物Tert-butyl 4-fluorobenzoateHCID 2736444—
溶媒Dimethyl SulfoxideHCID 679—
溶媒WaterHCID 962—
生成物4-[2-(Dimethylamino)ethylthio]-benzoic acidHCID 16787219110.3%

反応条件

温度80 °C

反応手順

A suspension of tert-butyl 4-fluorobenzoate (300 mg), 2-(dimethylamino)-ethanethiol hydrochloride (420 mg), and potassium carbonate (620 mg) in dimethylsulfoxide (3.0 mL) is stirred at 80° C. for 4 hours. The reaction mixture is diluted with water and extracted with ethyl acetate. The extract is concentrated in vacuo and to the residue is added 4N HCl-dioxane (1.5 mL). The mixture is stirred at room temperature overnight. The reaction mixture is diluted with ether and the precipitated crystals are collected by filtration to give 4-[2-(dimethylamino)ethylthio]-benzoic acid (380 mg, yield; 99%) as colorless crystals. MS (APCI) m/z; 226 [M+H]+

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07384952B2
出典データセットuspto-grants-2008_06
ORD IDord-a153716750a84def84a3a8d919f29795
出典メモuspto-grants-2008_06