反応 #62356

反応方程式

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

収率 75.4%

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

収率 75.4%

溶媒

water

ethyl acetate

反応条件

後処理

1. 1
   workup.STIRRINGstirred at this temperature for a day
2. 2
   洗浄the organic layer was washed successively with saturated aqueous ammonium chloride and saturated brine
3. 3
   乾燥dried over anhydrous magnesium sulfate
4. 4
   その他the solvent was evaporated
5. 5
   その他The residue was purified
6. 6
   その他separated by silica gel column chromatography (ethyl acetate:n-hexane=1:30)

実験手順

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.

出典