反応 #62408

反応方程式

trityl-chloride

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

sodium hydride

water

→

title compound

収率 73.9%

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

収率 73.9%

溶媒

N,N-dimethylformamide

ethyl acetate

反応条件

後処理

1. 1
   洗浄washing successively with aqueous ammonium chloride and saturated brine
2. 2
   乾燥drying over anhydrous magnesium sulfate
3. 3
   その他the solvent was evaporated
4. 4
   その他The residue was purified
5. 5
   その他separated 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
   洗浄Then the precipitated crystals were washed with diethyl ether

実験手順

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.

出典