Реакция #62345

Уравнение реакции

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

diisopropylethylamine

trityl chloride

→

title compound

Выход 47.3%

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

Выход 47.3%

Растворители

dichloromethane

Условия реакции

Обработка

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

Методика

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.

Источник