반응 #62345

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3-iodo-1H-pyrazolo[3,4-c]pyridine-5-carbonitrile

diisopropylethylamine

trityl chloride

→

title compound

수율 47.3%

3-Iodo-1-trityl-1H-pyrazolo[3,4-c]pyridine-5-carbonitrile

수율 47.3%

용매

dichloromethane

반응 조건

후처리

1. 1
   기타The solution was evaporated
2. 2
   workup.ADDITIONdiluted with ethyl acetate
3. 3
   세척washed successively with saturated ammonium chloride and saturated brine
4. 4
   건조dried over anhydrous magnesium sulfate
5. 5
   기타The solvent was evaporated
6. 6
   기타the crude product was purified
7. 7
   기타separated by silica gel column chromatography (ethyl acetate:n-hexane=1:10)

실험 절차

To a solution of 5.8 g of 3-iodo-1H-pyrazolo[3,4-c]pyridine-5-carbonitrile in 70 mL of dichloromethane were added 13.1 mL of diisopropylethylamine, 2.4 g of tetra-n-butylammonium iodide and 12.0 g of trityl chloride at room temperature, and stirred at this temperature for a day. The solution was evaporated, diluted with ethyl acetate, washed successively with saturated ammonium chloride and saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated, and the crude product was purified and separated by silica gel column chromatography (ethyl acetate:n-hexane=1:10), to afford 5.2 g of the title compound as colorless crystals.

출처