17216-62-5, Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 17216-62-5, name is Diethyl 2-(2-cyanoethyl)malonate, A new synthetic method of this compound is introduced below.
241 kg of the above intermediate, 1200 kg of isopropyl alcohol and 28 kg of catalyst Raney Co were placed in a 2-liter stainless steel autoclave. After replacing the air in the kettle with hydrogen,Press the hydrogen pressure to 25kg/cm2, turn on the stirring, and slowly raise the temperature to 70 C with jacketed steam.Above, the oxygen inhalation reaction begins to exotherm. At this point, turn on the cooling water to cool.The reaction temperature was controlled to rise smoothly to 90-100 C, and the introduction of hydrogen gas was controlled to stabilize the pressure at 35-40 kg/cm 2 .After 4.5 hours, the hydrogen absorption was stopped and the reaction was continued at 100 C, 35 kg / cm 2 for 1 hour.The material in the autoclave was cooled to 44 C with cooling water, and after the residual hydrogen pressure was vented,Press the material to the filter with N2 gas.The Raney Co catalyst was recovered by filtration under N2 gas protection.The filtrate was introduced into a 2000 liter glass-line distillation crystallization kettle, and heated under stirring.The solvent isopropanol was distilled off. Then add 660 kg of petroleum ether while stirring for 0.5 hour.The crystals are gradually cooled, and the stirring is intermittently started to prevent the product from being easily discharged from the bottom of the kettle after agglomeration. After the completion of the crystallization, the mixture was centrifuged and dried to give 184 kg of a white solid. The content of HPLC detection was 99.6%, and the hydrogenation reaction yield was 96.4%.The total yield of the two-step reaction was 79.2%.
The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.
Reference:
Patent; Shanghai Jingwei Chemical Technology Co., Ltd.; Yao Husheng; Zhao Zhulin; Zhang Ming; Chen Bo; (6 pag.)CN108484484; (2018); A;,
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