Reference of 348640-02-8, In the chemical reaction process,reaction time,type of solvent,can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product.An updated downstream synthesis route of 348640-02-8 as follows.
A solution of 209-2 (50.0 g, 183.8 mmol) in dry THF cooled to -78 C. and n-BuLi (81 ml, 2.5 M in hexane) was added over 20 minutes. The resulted solution was maintained at -78 C. for 1 h, and then a solution of BrCl2CCCl2Br (71.0 g, 220.5 mmol) in dry THF was added. The mixture was stirred -78 C. for 30 min and allowed to warm slowly to room temperature. The solvent was removed under vacuum and the residue was partitioned between EtOAc and water. The organic layer was dried over anhydrous Na2SO4 and concentrated. The crude product was purified by column chromatography (5% ethyl acetate in petroleum ether to 20% ethyl acetate in petroleum ether as the eluent) to afford 209-3 (37 g, 58% yield). MS-ESI: m/z=351.0 [M+1]+
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,348640-02-8, its application will become more common.
Reference:
Patent; INTERMUNE, INC.; US2009/318455; (2009); A1;,
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