Reaktion #62345

Reaktionsgleichung

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

diisopropylethylamine

trityl chloride

→

title compound

Ausbeute 47.3%

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

Ausbeute 47.3%

Lösungsmittel

dichloromethane

Reaktionsbedingungen

Aufarbeitung

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

Vorschrift

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.

Quelle