Synthetic Route of 658-99-1,Some common heterocyclic compound, 658-99-1, name is 2-(3,4-Difluorophenyl)acetonitrile, molecular formula is C8H5F2N, 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.
General procedure: To a stirring solution of substituted benzonitrile/phenylacetonitrile (1mmol) in anhydrous methanol (20mL) under N2 atmosphere was added hydroxylamine hydrochloride (1.2mmol). Triethylamine (2.5mmol) was added under continuous stirring condition and the mixture was then heated under reflux condition for overnight at 60C and continued until complete consumption of the starting material (monitored by TLC) [22,23]. The excess solvent was then removed under reduced pressure and the obtained residue was washed successively with water and brine, and extracted with ethylacetate (3×10mL). The organic layer was dried over anhydrous Na2SO4 and concentrated under reduced pressure. This reaction mixture was purified using silica gel column chromatography with a gradient solvent system of 10-20% ethylacetate to hexane to obtain the desired product with an average yield of 70-80%.
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2-(3,4-Difluorophenyl)acetonitrile, its application will become more common.
Reference:
Article; Paul, Saurav; Roy, Ashalata; Deka, Suman Jyoti; Panda, Subhankar; Trivedi, Vishal; Manna, Debasis; European Journal of Medicinal Chemistry; vol. 121; (2016); p. 364 – 375;,
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