تفاعل #62356

معادلة التفاعل

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

المردود 75.4%

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

المردود 75.4%

المذيبات

water

ethyl acetate

ظروف التفاعل

المعالجة

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

الإجراء التجريبي

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.

المصدر