Reacción #62356

Ecuación de reacción

trityl chloride

5-iodo-3-(naphthalen-2-yl)-1H-thieno[2,3-c]pyrazole

N,N-dimethylformamide

1H-Thieno[2,3-c]pyrazole-5-carbonitrile

sodium hydride

→

title compound

Rendimiento 75.4%

5-Iodo-3-(naphthalen-2-yl)-1-trityl-1H-thieno[2,3-c]-pyrazole

Rendimiento 75.4%

Disolventes

water

ethyl acetate

Condiciones de reacción

Tratamiento posterior

1. 1
   workup.STIRRINGstirred at this temperature for a day
2. 2
   Lavadothe organic layer was washed successively with saturated aqueous ammonium chloride and saturated brine
3. 3
   Secadodried over anhydrous magnesium sulfate
4. 4
   Otrothe solvent was evaporated
5. 5
   OtroThe residue was purified
6. 6
   Otroseparated by silica gel column chromatography (ethyl acetate:n-hexane=1:30)

Procedimiento

To a solution of 75 mg of 5-iodo-3-(naphthalen-2-yl)-1H-thieno[2,3-c]pyrazole in 1 m L of N,N-dimethylformamide 1 was added 12 mg of sodium hydride at room temperature, stirred for 15 minutes, then added with 56 mg of trityl chloride, and stirred at this temperature for a day. The solution was added with water and diluted with ethyl acetate, and the organic layer was washed successively with saturated aqueous ammonium chloride and saturated brine, dried over anhydrous magnesium sulfate, and the solvent was evaporated. The residue was purified and separated by silica gel column chromatography (ethyl acetate:n-hexane=1:30), to afford 93 mg of the title compound as colorless crystals.

Fuente