Electric Literature of 1897-52-5, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 1897-52-5 name is 2,6-Difluorobenzonitrile, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.
Cyano-(2-cyano-3-fluoro-phenyl)-acetic acid ethyl ester.A mixture of cyanoacetic acid ethyl ester (26.7 mL, 251 mmol), 2,6-difluorobenzonitrile (33.2 g, 239 mmol) and potassium carbonate (82.5 g, 597 mmol) in dimethyl sulfoxide (120 mL) was stirred at +55C for 16 hours and poured into ice-water mixture (ca. 400 mL). It was acidified with cone. aq. HCl with caution (CO2 evolution) and extracted with ethyl acetate (600 ml). The organic phase was washed with brine (100 mL) and evaporated to give 55.1 g of a pale yellow solid that was used in the next step without further purification. 1H NMR (500 MHz, CDCl3): 1.35 (t, J=7.0 Hz, 3H), 4.34 (m, 2H), 5.13 (s, IH), 7.33 (t, J=8.4 Hz, IH), 7.57 (d, J=7.9 Hz, IH), 7.33 (dd, J=7.9 Hz, J=13.9 Hz, IH).
At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2,6-Difluorobenzonitrile, and friends who are interested can also refer to it.
Reference:
Patent; H. LUNDBECK A/S; WO2009/156339; (2009); A1;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts