反应详情

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.

1. washThe organic layer was washed successively with saturated aqueous ammonium chloride and saturated brine
2. dry with materialdried over anhydrous magnesium sulfate
3. customthe solvent was evaporated
4. customThe crude product was purified
5. customseparated by silica gel column chromatography (ethyl acetate:n-hexane=1:10)