Synthetic Route of 100367-55-3, 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. 100367-55-3, name is 5-Nitropicolinonitrile. A new synthetic method of this compound is introduced below.
4) 1864.7 g of reduced Fe powder was added to 16780 g of ethyl acetate and 1864.7 g of 2-cyano-5-nitropyridine,Oil bath heated to 81 began to drop 8299g of acetic acid, acetic acid was added dropwise to maintain a steady reflux, with the dropping of reflux temperature byGradually rise to 89 , and the need to be added within 310min was completed; after completion of the dropwise addition at 81 reaction temperature incubated for 5h.5) The reaction solution obtained in step 4) was filtered while hot at 65 C, the filtrate, the filter cake separately treated, wherein the filtrate withNaOH temperature was controlled at 5 ~ 10 , pH adjusted to 8.5, with ethyl acrylate back to the aqueous phase; to the filter cake was added the amount of propyleneEthyl acetate and NaHSO3 aqueous solution, warmed to 60 C, stirred for 15min and filtered, again with ethyl acrylate back to the aqueous phase; mergeThe organic phase obtained above was washed with saturated NaCl solution and then concentrated. Finally, 1270 g of tan solid B, 2-cyano-5-Aminopyridine, yield 85.3%, purity 97%.
At the same time, in my other blogs, there are other synthetic methods of this type of compound,100367-55-3, 5-Nitropicolinonitrile, and friends who are interested can also refer to it.
Reference:
Patent; Silver Yunxin Biological Technology Co., Ltd.; Pan Jincheng; Li Shoude; Pan Shangguang; (7 pag.)CN106810494; (2017); A;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem