反应详情

温度

40 °C

To a solution of 70 mg of 3-naphthalene-2-yl-1H-thieno[2,3-c]pyrazole obtained by Example 78 in 3.0 mL of N,N-dimethylformamide was added 63 mg of N-iodosuccinimide at room temperature, and stirred at 40° C. for a day. Then the solution was added with 1.0 mL of 10% sodium thiosulfate aqueous solution, and extracted 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. The crude product was purified and separated by silica gel column chromatography (ethyl acetate:n-hexane=1:3), to afford 75 mg of the title compound as colorless crystals.

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