反应 #62355

反应方程式

sodium thiosulfate

3-naphthalene-2-yl-1H-thieno[2,3-c]pyrazole

3-(Naphthalen-2-yl)-1H-thieno[2,3-c]pyrazole

N-iodosuccinimide

→

title compound

收率 71.3%

5-Iodo-3-(naphthalen-2-yl)-1H-thieno[2,3-c]pyrazole

收率 71.3%

溶剂

N,N-dimethylformamide

反应条件

后处理

1. 1
   萃取extracted with ethyl acetate
2. 2
   洗涤The organic layer was washed successively with saturated aqueous ammonium chloride and saturated brine
3. 3
   干燥dried over anhydrous magnesium sulfate
4. 4
   其他the solvent was evaporated
5. 5
   其他The crude product was purified
6. 6
   其他separated by silica gel column chromatography (ethyl acetate:n-hexane=1:3)

实验过程

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.

来源