Electric Literature of 939-79-7,Some common heterocyclic compound, 939-79-7, name is 4-Methyl-3-nitrobenzonitrile, molecular formula is C8H6N2O2, 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: The reaction materials were 2-nitro-4-cyanotoluene (162 mg, 1 mmol), butyl methacrylate (430 mg, 3 mmol) for 8 hours, and the specific operation was the same as in Example 1. The product was a white solid, yield 158 mg, yield 58%.;_A 10 mL round bottom flask equipped with a reflux condenser was charged with 2,4-dinitrotoluene (182 mg, 1 mmol). methyl methacrylate (294 mg, 3 mmol) and cesium carbonate (652 mg, 2 mmol). Nitrogen was bubbled through anhydrous THF (5 mL), heated to 65 C and refluxed for 12 hours. After the end of the reaction, the solvent is removed by rotary evaporation and the excess olefin is removed. The residual solid is washed with sufficient amount of methylene chloride, filtered, the residue is dissolved in sufficient water. After removal of the solid, the solvent was dried and dried in vacuo to give recovered cesium carbonate. The filtrate containing the product was spin-dried and purified by silica gel column eluting with dichloromethane to give the title product as a yellow solid, yield 213 mg, yield 85%.
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 4-Methyl-3-nitrobenzonitrile, its application will become more common.
Reference:
Patent; Tianjin Normal University; Liu, Guiyan; Wang, Jianhui; Yin, Maocong; Liu, Chengxin; (11 pag.)CN106397317; (2017); A;,
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