With the rapid development and complex challenges of chemical substances, the synthesis of new drugs is usually one of the most effective ways to increase yield.97483-77-7, name is 5-Bromopicolinonitrile, molecular formula is C6H3BrN2, molecular weight is 183.01, as common compound, the synthetic route is as follows.Quality Control of 5-Bromopicolinonitrile
A solution of 5-bromo-2-pyridinecarbonitrile (2.0 g, 10.9 mmol) in dichloromethane (75 mL) was cooled to -78 degrees C., then a solution of DIBAL in toluene (1.5 M, 7.3 mL, 10.9 mmol) was added dropwise, taking care to keep the temperature below -65 degrees C. The resulting orange solution was stirred at -78 degrees C. for 5 h, then was allowed to gradually warm to 0 degrees C. The reaction was cooled back to -78 degrees C., then was quenched by dropwise addition of 20% aq. HCl. After warming to room temperature, the organic layer was separated, concentrated in vacuo and purified by chromatography to provide the product. The aqueous layer was treated with solid sodium bicarbonate until neutral, then this emulsion was extracted with ethyl acetate (3¡Á). These extracts were dried over sodium sulfate and concentrated in vacuo to provide additional product, 5-bromo-2-pyridinecarbaldehyde. 1H NMR (400 MHz, CDCl3) delta 7.85 (d, J=8.18 Hz, 1H), 8.02 (d, J=8.18 Hz, 1H), 8.85 (s, 1H), 10.03 (s, 1H).
At the same time, in my other blogs, there are other synthetic methods of this type of compound,97483-77-7, 5-Bromopicolinonitrile, and friends who are interested can also refer to it.
Reference:
Patent; Diaz, Caroline Jean; Haffner, Curt Dale; Speake, Jason Daniel; Zhang, Cunyu; Mills, Wendy Yoon; Spearing, Paul Kenneth; Cowan, David John; Green, Gary Martin; US2010/222345; (2010); A1;,
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