反応 #62301

反応方程式

ethyl acetate

water

5-bromo-2,3-difluorobenzaldehyde

copper cyanide

→

title compound

収率 42.9%

3,4-Difluoro-5-formylbenzonitrile

収率 42.9%

溶媒

1-methyl-2-pyrrolidone

反応条件

後処理

1. 1
   ろ過insoluble substances were filtered out through celite
2. 2
   洗浄The organic layer of filtrate was washed successively with saturated aqueous ammonium chloride, water and saturated brine
3. 3
   乾燥dried over anhydrous magnesium sulfate
4. 4
   その他the solvent was evaporated
5. 5
   その他The crude product was purified
6. 6
   その他separated by silica gel column chromatography (ethyl acetate:n-hexane=1:20)

実験手順

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.

出典