반응 #62354

반응 방정식

sodium thiosulfate

1H-thieno[2,3-c]pyrazole 5-carbonitrile

N-bromosuccinimide

→

title compound

수율 85.8%

3-Bromo-1H-thieno[2,3-c]pyrazole-5-carbonitrile

수율 85.8%

용매

ethyl acetate

dimethylformamide

반응 조건

후처리

1. 1
   세척The organic layer was washed successively with saturated aqueous ammonium chloride and saturated brine
2. 2
   건조dried over anhydrous magnesium sulfate
3. 3
   기타the solvent was evaporated
4. 4
   기타The crude product was purified
5. 5
   기타separated by silica gel column chromatography (ethyl acetate:n-hexane=1:10)

실험 절차

To a solution of 168 mg of 1H-thieno[2,3-c]pyrazole 5-carbonitrile in 5 mL of dimethylformamide was added 200 mg of N-bromosuccinimide at room temperature and stirred at this temperature for 2 hours. After adding 1 mL of 10% sodium thiosulfate aqueous solution, the solution was diluted with ethyl acetate. The organic layer was washed successively with saturated aqueous ammonium chloride and saturated brine, dried over anhydrous magnesium sulfate, and the solvent was evaporated. This afforded 3.7 g of the title compound as a colorless oil. The crude product was purified and separated by silica gel column chromatography (ethyl acetate:n-hexane=1:10), to afford 220 mg of the title compound as colorless crystals.

출처