反応 #62345

反応方程式

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

diisopropylethylamine

trityl chloride

→

title compound

収率 47.3%

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

収率 47.3%

溶媒

dichloromethane

反応条件

後処理

1. 1
   その他The solution was evaporated
2. 2
   workup.ADDITIONdiluted with ethyl acetate
3. 3
   洗浄washed successively with saturated ammonium chloride and saturated brine
4. 4
   乾燥dried over anhydrous magnesium sulfate
5. 5
   その他The solvent was evaporated
6. 6
   その他the crude product was purified
7. 7
   その他separated by silica gel column chromatography (ethyl acetate:n-hexane=1:10)

実験手順

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.

出典