반응 #62408

반응 방정식

trityl-chloride

5-bromo-6-fluoro-3-iodo-1H-indazole

sodium hydride

water

→

title compound

수율 73.9%

5-Bromo-6-fluoro-3-iodo-1-trityl-1H-indazole

수율 73.9%

용매

N,N-dimethylformamide

ethyl acetate

반응 조건

후처리

1. 1
   세척washing successively with aqueous ammonium chloride and saturated brine
2. 2
   건조drying over anhydrous magnesium sulfate
3. 3
   기타the solvent was evaporated
4. 4
   기타The residue was purified
5. 5
   기타separated by silica gel column chromatography (ethyl acetate:n-hexane=1:30-1:5)
6. 6
   workup.ADDITIONthe resultant product was added with n-hexane
7. 7
   세척Then the precipitated crystals were washed with diethyl ether

실험 절차

To a solution of 3.0 g of 5-bromo-6-fluoro-3-iodo-1H-indazole in N,N-dimethylformamide in 150 mL was added 0.42 g of sodium hydride at room temperature, and the resultant solution was stirred for 15 minutes, added with 2.45 g of trityl-chloride, and stirred at this temperature for 1 hour. After adding water and diluting with ethyl acetate, washing successively with aqueous ammonium chloride and saturated brine and drying over anhydrous magnesium sulfate, the solvent was evaporated. The residue was purified and separated by silica gel column chromatography (ethyl acetate:n-hexane=1:30-1:5), and the resultant product was added with n-hexane. Then the precipitated crystals were washed with diethyl ether:n-hexane=1:10, to afford 3.79 g of the title compound as colorless crystals.

출처