반응 #62356

반응 방정식

trityl chloride

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

N,N-dimethylformamide

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

sodium hydride

→

title compound

수율 75.4%

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

수율 75.4%

용매

water

ethyl acetate

반응 조건

후처리

1. 1
   workup.STIRRINGstirred at this temperature for a day
2. 2
   세척the organic layer was washed successively with saturated aqueous ammonium chloride and saturated brine
3. 3
   건조dried over anhydrous magnesium sulfate
4. 4
   기타the solvent was evaporated
5. 5
   기타The residue was purified
6. 6
   기타separated by silica gel column chromatography (ethyl acetate:n-hexane=1:30)

실험 절차

To a solution of 75 mg of 5-iodo-3-(naphthalen-2-yl)-1H-thieno[2,3-c]pyrazole in 1 m L of N,N-dimethylformamide 1 was added 12 mg of sodium hydride at room temperature, stirred for 15 minutes, then added with 56 mg of trityl chloride, and stirred at this temperature for a day. The solution was added with water and diluted with ethyl acetate, and 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 residue was purified and separated by silica gel column chromatography (ethyl acetate:n-hexane=1:30), to afford 93 mg of the title compound as colorless crystals.

출처