反应详情

Trityl chloride (885 mg, 3.2 mmol) was added to a stirred cold (0-5° C.) solution of 4-iodo pyrazole (513 mg, 2.6 mmol) and triethylamine (401 mg, 0.55 mL, 0.4 mmol) in DCM (10 mL). Stirring was continued at room temperature overnight. Cold water was then added and the product was extracted with DCM and the organic layer was washed with sat. sodium bicarbonate solution followed by brine. The organic phase was dried over Na2SO4 and concentrated under reduced pressure to get the residue. The obtained residue was purified by column chromatography (using neutral alumina and 2% EtOAc in Hexane as eluent) to afford 300 mg (26% yield) of 4-iodo-1-trityl-1H-pyrazole.

1. extractionthe product was extracted with DCM
2. washthe organic layer was washed with sat. sodium bicarbonate solution
3. dry with materialThe organic phase was dried over Na2SO4
4. concentrationconcentrated under reduced pressure
5. customto get the residue
6. customThe obtained residue was purified by column chromatography (using neutral alumina and 2% EtOAc in Hexane as eluent)