تفاعل #62301

معادلة التفاعل

ethyl acetate

water

5-bromo-2,3-difluorobenzaldehyde

copper cyanide

→

title compound

المردود 42.9%

3,4-Difluoro-5-formylbenzonitrile

المردود 42.9%

المذيبات

1-methyl-2-pyrrolidone

ظروف التفاعل

المعالجة

1. 1
   ترشيحinsoluble substances were filtered out through celite
2. 2
   غسيلThe organic layer of filtrate was washed successively with saturated aqueous ammonium chloride, water and saturated brine
3. 3
   تجفيفdried over anhydrous magnesium sulfate
4. 4
   أخرىthe solvent was evaporated
5. 5
   أخرىThe crude product was purified
6. 6
   أخرىseparated by silica gel column chromatography (ethyl acetate:n-hexane=1:20)

الإجراء التجريبي

To a solution of 10.0 g of 5-bromo-2,3-difluorobenzaldehyde in 40.0 mL of 1-methyl-2-pyrrolidone was added 4.26 g of copper cyanide (I) at room temperature and stirred at 170° C. for 8 hours. Adding ethyl acetate and water, the solution was stirred, and insoluble substances were filtered out through celite. The organic layer of filtrate was washed successively with saturated aqueous ammonium chloride, water and saturated brine, dried over anhydrous magnesium sulfate, and the solvent was evaporated. The crude product was purified and separated by silica gel column chromatography (ethyl acetate:n-hexane=1:20), to afford 2.64 g of the title compound as colorless crystals.

المصدر