반응 #437930

반응 방정식

3-[2-amino-4-(4-chlorophenyl)-5-thiazolyl]propionic acid

diethyl cyanophosphate

thiomorpholine-1,1-dioxide hydrochloride

triethylamine

→

4-{3-[2-amino-4-(4-chlorophenyl)-5-thiazolyl]propanoyl}thiomorpholine-1,1-dioxide

용매

N,N-dimethylformamide

water

반응 조건

후처리

1. 1
   추출extracted with ethyl acetate
2. 2
   세척washed with 0.1N aqueous sodium hydroxide solution and water
3. 3
   건조dried over anhydrous magnesium sulfate
4. 4
   농축concentrated
5. 5
   여과The precipitated solid was collected by filtration

실험 절차

A mixture of 3-[2-amino-4-(4-chlorophenyl)-5-thiazolyl]propionic acid (2.67 g), diethyl cyanophosphate (1.69 g), thiomorpholine-1,1-dioxide hydrochloride (1.62 g), triethylamine (2.9 ml) and N,N-dimethylformamide (40 ml) was stirred at room temperature for 3 hrs. The reaction mixture as poured into water, extracted with ethyl acetate, washed with 0.1N aqueous sodium hydroxide solution and water, dried over anhydrous magnesium sulfate and concentrated. The precipitated solid was collected by filtration to give 4-{3-[2-amino-4-(4-chlorophenyl)-5-thiazolyl]propanoyl}thiomorpholine-1,1-dioxide as a colorless powder. Recrystallization from ethanol-isopropyl ether gave colorless prism crystals. melting point: 220–222° C.

출처