تفاعل #62354

معادلة التفاعل

sodium thiosulfate

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

N-bromosuccinimide

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title compound

المردود 85.8%

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

المردود 85.8%

المذيبات

ethyl acetate

dimethylformamide

ظروف التفاعل

المعالجة

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

الإجراء التجريبي

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.

المصدر