反応 #72075

反応方程式

2,4-Dinitrobenzonitrile

Potassium carbonate

ethyl thioglycolate

→

title compound

収率 32.4%

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

収率 32.4%

溶媒

DMF

反応条件

後処理

1. 1
   濃縮The reaction solution was concentrated under reduced pressure
2. 2
   workup.ADDITIONdiluted with ethyl acetate
3. 3
   洗浄washed with water
4. 4
   乾燥dried over anhydrous sodium sulfate
5. 5
   濃縮concentration under reduced pressure
6. 6
   その他the residue was recrystallized from ethyl acetate/hexane

実験手順

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%).

出典