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. 641571-11-1, name is 3-(4-Methyl-1H-imidazol-1-yl)-5-(trifluoromethyl)aniline, A new synthetic method of this compound is introduced below., category: imidazoles-derivatives
To 400 mL of N-methyl-2-pyrrolidone, 80.0 g (261 mmol) of compound [1] and 0.43 g (5.2 mmol) of cyclohexene were added, and 43.5 g (366 mmol) of thionyl chloride was added dropwise at 20 to 40 C., followed by 60 C. The temperature was raised and the reaction was carried out for 1 hour. After confirming the reaction end point, a solution prepared by dissolving 63.0 g (261 mmol) of compound [3] in 400 mL of N-methyl-2-pyrrolidone was added dropwise to the reaction mass, and the mixture was reacted at 60 C. for 3 hours. After 400 mL of water was introduced into the reaction mass, the temperature was raised to 80 C, 83.0 g of a 20% KOH aqueous solution was added dropwise, and the temperature was kept at 80 C for 3 hours or more.Subsequently, 112.3 g of a 20% KOH aqueous solution was added dropwise over 1 h. After cooling to 60 C., 45.2 g of a 40% K 2 CO 3 aqueous solution was added dropwise, and the mixture was cooled to 40 C. over about 2 hours. The obtained crystals were dried under reduced pressure to obtain 128.6 g of compound [4] (nilotinib) (yield 93.0%). The area percentage of the peak of the target substance in the LC chromatogram was 99.96% (nuclear chlorinated product was not detected).
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; Sumitomo Chemical Co., Ltd.; Kumazawa, Hiroharu; Akiyama, Masaki; (8 pag.)JP2020/7240; (2020); A;,
Imidazole – Wikipedia,
Imidazole | C3H4N2 – PubChem