Synthetic Route of 64248-64-2,Some common heterocyclic compound, 64248-64-2, name is 2,5-Difluorobenzonitrile, molecular formula is C7H3F2N, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
Step A: Thio-Amide Synthesis:1-1 1 -2A stirred solution of the appropriate benzonitrile e.g., 2,5-difluorobenzonitrile (1-1), (15 mmol) in pyridine (10 rnL) was treated with sulfide (20% wt solution in water, 16.5 mmol) and triethyl amine (16.5 mmol). The reaction mixture was stirred at 500C for 5 hr until the reaction was complete. After cooling to RT, the mixture was diluted with cold water. Extracted with EtOAc, and the organics separated, then washed with H2O (x3), sat. brine (x3), then dried (Na2SO4), filtered, and evaporated under reduced pressure to give the crude. Purification on silica gel column (20% ethyl acetate/hexane) to afford thio-amide as yellow solid, 1-2 (yield 88.5%). 1H NMR (300 MHz, CDCl3): delta 7.12 (m, 2 H), 7.90 (br, 2 H), 8.08 (m, 1 H).
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2,5-Difluorobenzonitrile, its application will become more common.
Reference:
Patent; NOVARTIS AG; WO2008/63912; (2008); A1;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts