Reacción #62345
ord-ece1696588f2407289d727effe25fd70
Ecuación de reacción
3-iodo-1H-pyrazolo[3,4-c]pyridine-5-carbonitrile
diisopropylethylamine
trityl chloride
→
title compound
Rendimiento 47.3%
3-Iodo-1-trityl-1H-pyrazolo[3,4-c]pyridine-5-carbonitrile
Rendimiento 47.3%
Reactivos
Disolventes
Condiciones de reacción
Condiciones detalladas
See reaction.notes.procedure_details.
Tratamiento posterior
- 1OtroThe solution was evaporated
- 2workup.ADDITIONdiluted with ethyl acetate
- 3Lavadowashed successively with saturated ammonium chloride and saturated brine
- 4Secadodried over anhydrous magnesium sulfate
- 5OtroThe solvent was evaporated
- 6Otrothe crude product was purified
- 7Otroseparated by silica gel column chromatography (ethyl acetate:n-hexane=1:10)
Procedimiento
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.