Synthetic Route of 4513-77-3, These common heterocyclic compound, 4513-77-3, name is 2-Oxocyclohexanecarbonitrile, its 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.
To a solution of triphenylphosphine (29.9 g, 114 mmol) in 500 ml_ of THF, cooled to 0 0C, was slowly added a 40% solution of diethyl azodicarboxylate in toluene (52.2 ml_, 114 mmol), ethyl glycolate (10.8 ml_, 114 mmol) and 2- oxocyclohexanecarbonitrile (10 g, 81.3 mmol). The resulting solution was stirred at room temperature for 20 hours. Then 50% sodium hydride (11 g, 229 mmol) was added and the mixture was stirred at room temperature for 5 hours. The reaction mixture was cooled to 0 0C and a pH 7.8 phosphate buffer (Na2HPO4/KH2PO4) solution (375 ml_) was added. THF was evaporated and the resulting aqueous solution was extracted with EtOAc. The organic phase was dried over Na2SO4 and concentrated to dryness. The resulting crude product was chromatographed on silica gel using hexane/EtOAc mixtures of increasing polarity as eluent, to afford 8.5 g of the desired compound (yield: 50%).
Statistics shows that 2-Oxocyclohexanecarbonitrile is playing an increasingly important role. we look forward to future research findings about 4513-77-3.
Reference:
Patent; PALAU PHARMA, S. A.; WO2009/56551; (2009); A1;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts