반응 #72075

반응 방정식

2,4-Dinitrobenzonitrile

Potassium carbonate

ethyl thioglycolate

→

title compound

수율 32.4%

Ethyl 3-amino-6-nitro-1-benzothiophene-2-carboxylate

수율 32.4%

용매

DMF

반응 조건

후처리

1. 1
   농축The reaction solution was concentrated under reduced pressure
2. 2
   workup.ADDITIONdiluted with ethyl acetate
3. 3
   세척washed with water
4. 4
   건조dried over anhydrous sodium sulfate
5. 5
   농축concentration under reduced pressure
6. 6
   기타the residue was recrystallized from ethyl acetate/hexane

실험 절차

2,4-Dinitrobenzonitrile (5.08 g, 26.3 mmol) was dissolved in DMF (55 ml). Potassium carbonate (4.36 g, 31.6 mmol) and ethyl thioglycolate (3.17 g, 26.3 mmol) were added, and the mixture was stirred at room temperature for three days. The reaction solution was concentrated under reduced pressure, diluted with ethyl acetate, washed with water, and dried over anhydrous sodium sulfate. Following concentration under reduced pressure, the residue was recrystallized from ethyl acetate/hexane to obtain 2.27 g of the title compound as crystals (32%).

출처