Application of 13958-99-1, 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. 13958-99-1, name is 3-Bromoisonicotinamide. A new synthetic method of this compound is introduced below.
3- Bromo-4-cyanopyridine (34). 3-Bromopyridine-4-carboxamide98 (687 mg, 3.4 mmol) was added to phosphorus oxychloride (5.0 ml_) at 0C. The mixture was then stirred at reflux for 2 h. The mixture was cooled, poured onto ice (100 g) with stirring and was neutralised with aqueous sodium hydroxide (5 M, 60 ml_). The mixture was extracted with diethyl ether (2 chi 50 mL). The combined organic layers were washed with saturated aqueous sodium hydrogen carbonate, treated with charcoal and filtered. The solvent was evaporated. The solid was recrystallised from petroleum ether to give 34 (292 mg, 42%) as an off-white powder: mp 79-81 C (lit.99 mp 96.6-98.2C); 1H NMR (CDCI3) delta 7.53 (1 H, d, J = 4.9 Hz, 5-H), 8.69 (1 H, d, J = 4.9 Hz, 6-H), 8.92 (1 H, s, 2- H); 13C NMR (CDCI3) (HSQC / HMBC) delta 1 14.79 (C?N), 122.14 (4-C), 124.17 (3-C), 126.75 (5-C), 148.76 (6-C), 152.69 (2-C); MS (ESI) m/z 182.9552 (M + H) (C6H4N279Br requires 182.9541).
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,13958-99-1, its application will become more common.
Reference:
Patent; UNIVERSITY OF BATH; THREADGILL, Michael David; LLOYD, Matthew David; THOMPSON, Andrew Spencer; NATHUBHAI, Amit; WOOD, Pauline Joy; PAINE, Helen Angharad; KUMPAN, Ekaterina; SUNDERLAND, Peter Thomas; CHUE YEN WOON, Esther; WO2014/87165; (2014); A1;,
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