In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 2369-19-9, name is 2-Fluoro-5-methylpyridine, the common compound, a new synthetic route is introduced below. Recommanded Product: 2369-19-9
(1) Synthesis of 2-fluoro-3-iodo-5-methylpyridine A 2.69 M n-butyllithium hexane solution (224 mL) was added dropwise to a mixture of diisopropylamine (92 mL) and THF (1.2 L) at -18C under a nitrogen atmosphere. Upon completion of the dropwise addition, the mixture was stirred while raising the temperature to -5C over a period of 20 minutes. The reaction mixture was cooled to -73C, and then a solution of 2-fluoro-5-methylpyridine (61 g) in THF (240 mL) was added dropwise thereto. The reaction mixture was stirred at -75C for 3.5 hours. A solution of iodine (139 g) in THF (24 mL) was added dropwise to the reaction mixture. The reaction mixture was stirred at -75C for 1 hour and 55 minutes. Upon completion of the reaction, water (220 mL) was added to the reaction mixture at the same temperature. The mixture was stirred for 5 minutes at the same temperature. The reaction mixture was warmed to room temperature, and then water (1.2 L) was added. An aqueous sodium thiosulfate pentahydrate (136 g) solution (300 mL) and water (300 mL) were added to the mixture, and the resultant was stirred for 10 minutes. The mixture was extracted with MTBE (1.2 L). The organic layer was washed with brine (500 mL). The combined aqueous layer was extracted with MTBE (1 L). The combined organic layer was dried over anhydrous magnesium sulfate. The desiccant was filtered out, and the filtrate was concentrated under reduced pressure. After adding n-heptane to the residue, the mixture was cooled. The precipitated solid was filtered out, and then was rinsed with n-heptane. The filtrate was cooled and the precipitated solid was filtered out. This procedure was repeated 5 times to obtain the title compound (109.69 g). 1H-NMR (400 MHz, CDCl3) delta (ppm):2.29-2.31 (m, 3H), 7.93-8.14 (m, 2H). ESI-MS m/z 238 [M+H]+
The synthetic route of 2369-19-9 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Eisai R&D Management Co., Ltd.; NORIMINE, Yoshihiko; SATO, Nobuaki; ISHIHARA, Yuki; TAKEDA, Kunitoshi; (65 pag.)EP2982674; (2016); A1;,
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