反应详情

温度

80 °C

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]+

1. extractionextracted with ethyl acetate
2. concentrationThe extract is concentrated in vacuo and to the residue
3. additionis added 4N HCl-dioxane (1.5 mL)
4. stirringThe mixture is stirred at room temperature overnight
5. additionThe reaction mixture is diluted with ether
6. filtrationthe precipitated crystals are collected by filtration