تفاعل #62406

معادلة التفاعل

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

sodium hydroxide

→

title compound

المردود 88.7%

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

المردود 88.7%

المذيبات

hydrochloric acid

ethanol

ethyl acetate

ظروف التفاعل

المعالجة

1. 1
   غسيلThe organic layer was successively washed with water and saturated brine
2. 2
   تجفيفdried over anhydrous magnesium sulfate
3. 3
   أخرىthe solvent was evaporated
4. 4
   أخرىThe residue was purified
5. 5
   أخرىseparated by silica gel column chromatography (ethyl acetate:n-hexane=1:3)

الإجراء التجريبي

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.

المصدر