反応 #62406

反応方程式

1-(5-bromo-6-fluoro-indazol-1-yl)ethanone

sodium hydroxide

→

title compound

収率 88.7%

5-Bromo-6-fluoro-1H-indazole

収率 88.7%

溶媒

hydrochloric acid

ethanol

ethyl acetate

反応条件

後処理

1. 1
   洗浄The organic layer was successively washed with water and saturated brine
2. 2
   乾燥dried 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=1:3)

実験手順

To a solution of 22.5 g of 1-(5-bromo-6-fluoro-indazol-1-yl)ethanone in 250 mL of ethanol was added 20.0 mL of 5N sodium hydroxide aqueous solution at room temperature, and stirred at this temperature for 5 minutes. After neutralizing in 5N hydrochloric acid aqueous solution, the solution was diluted with ethyl acetate. The organic layer was successively washed with water and saturated brine, dried over anhydrous magnesium sulfate, and then the solvent was evaporated. The residue was purified and separated by silica gel column chromatography (ethyl acetate:n-hexane=1:3), to afford 16.7 g of the title compound as pale brown crystals.

出典