As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 15513-52-7, name is 2,6-Dimethyl-3-nitropyridine, molecular formula is C7H8N2O2, The compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below. Quality Control of 2,6-Dimethyl-3-nitropyridine
3-Nitro-2,6-lutidine (2.50 g, 16.5 mmol, 1 equiv.) was dissolved in 200 mL of argonpurged carbon tetrachloride. The reaction mixture was heated to 50 C under argon. AIBN (0.14 g, 0.83 mmol, 5 mol%) was added to the reaction mixture in one portion under constant stirring, followed by the addition of NBS (2.93 g, 16.5 mmol, 1 equiv.) in small portions over a period of 2 hours. The reaction mixture was further refluxed for 8 hours at constant stirring and under light irradiation. Once the reaction was complete, solvent was removed in vacuo producing a brownish residue. This residue was suspended in a mixture of methanol-dichloromethane, in which non-dissolved solids were removed by filtering through a Si02 plug (ca. 120 mL) using an eluent of methanol-dichloromethane (1:20 v/v). Fractions containing ii were combined and solvent was removed in vacuo. The resultant oil was subject to Si02 column chromatography using a mixture of ethyl acetate (gradient from 2% to 10%) in hexanes as an eluent. Fractions containing product were concentrated in vacuo producinganalytically pure ii. Yield: 0.41 g, 1.78 mmol, 11%. ?H NMR, 500 MHz (CDC13, ppm): oe =8.26 d (1H, Ar, J = 9 Hz), 7.47 d (1H, Ar, J = 9 Hz), 4.52 s (2H, CH2), 2.83 s (3H, CH3). ?3C NMR, 75 MHz (CDC13, ppm): oe = 160.46, 153.73, 144.66, 133.66, 121.61, 32.07, 23.84. ESIMS (mlz): [M+H], calculated: 231.0, found: 231.0.
With the rapid development of chemical substances, we look forward to future research findings about 15513-52-7.
Reference:
Patent; THE RESEARCH FOUNDATION FOR THE STATE UNIVERSITY OF NEW YORK UNIVERSITY AT BUFFALO; HEALTH RESEARCH, INC.; MORROW, Janet, R.; TSITOVICH, Pavel, B.; DORAZIO, Sarina, J.; OLATUNDE, Abiola, O.; SNYDER, Eric, M.; SPERNYAK, Joseph, A.; BURNS, Patrick; BOND, Christopher, J.; WO2015/38943; (2015); A1;,
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