Reaktion #62408

Reaktionsgleichung

trityl-chloride

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

sodium hydride

water

→

title compound

Ausbeute 73.9%

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

Ausbeute 73.9%

Lösungsmittel

N,N-dimethylformamide

ethyl acetate

Reaktionsbedingungen

Aufarbeitung

1. 1
   Waschenwashing successively with aqueous ammonium chloride and saturated brine
2. 2
   Trocknendrying over anhydrous magnesium sulfate
3. 3
   Sonstigethe solvent was evaporated
4. 4
   SonstigeThe residue was purified
5. 5
   Sonstigeseparated 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
   WaschenThen the precipitated crystals were washed with diethyl ether

Vorschrift

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.

Quelle