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. 22282-96-8, name is 2-Bromo-6-methyl-5-nitropyridine. A new synthetic method of this compound is introduced below., Formula: C6H5BrN2O2
A suspension of 6-bromo-2-methyl-3-nitropyridine (XIV) (250 g, 1.15 mol, 1.00 eq) and NH4C1 (300 g, 5.61 mol, 4.88 eq) in EtOH (3.50 L) and water (150 mL) was heated with stirring to 65C. To this mixture was added Fe (130 g, 2.33 mol, 2.02 eq) and HQ (15.3 g, 419 mmol, 0.36 eq). The suspension was then heated to 80C for another 3 h. The reaction was cooled to 25C and filtered through a plug of Celite. The filtrate was concentrated under reduced pressure to yield a residue that was taken up in EtOAc (1 L x 3) and washed with brine. The organic layer was dried over sodium sulfate, filtered and concentrated under reduced pressure to give 6- bromo-2-methylpyridin-3-amine (XV) as brown solid (373 g, 1.99 mol, 86.7% yield) which was used for the next step without any purification. NMR (DMSO-de, 400 MHz) delta ppm 6.01 (dd, J = 2.3, 7.9 Hz, 2H), 7.03 (d, J= 8.2 Hz, IH); ESIMS found for C6H7BrN2 mlz 186.8 (M+H).
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Reference:
Patent; KC, Sunil Kumar; WALLACE, David Mark; CAO, Jianguo; CHIRUTA, Chandramouli; HOOD, John; (230 pag.)WO2017/24025; (2017); A1;,
Pyridine – Wikipedia,
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