Analyzing the synthesis route of 15513-52-7

With the rapid development of chemical substances, we look forward to future research findings about 15513-52-7.

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;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

The origin of a common compound about 15513-52-7

While traditionally a conservative industry, chemical producers will need to modernize their PR strategies to stay relevant.we look forward to future research findings about 15513-52-7, 2,6-Dimethyl-3-nitropyridine.

Electric Literature of 15513-52-7, The major producers of chemicals have been the Europe, Japan and China. Due to the growing call for a cleaner, greener environment, people will have to find innovative ways to maintain their relevance. Here is a compound 15513-52-7, name is 2,6-Dimethyl-3-nitropyridine. This compound has unique chemical properties. The synthetic route is as follows.

To a stirred solution of 2,6-dimethyl-3-nitropyridine (200mg, 1.3 mmol, 1.0 eq) in ethanol (10 mL) was added 40 % aqs. formaldehyde (15 mL) followed by water (10 mL) room temperature and stirred for 48 h at 200 C. The aqs solvent was evaporated and crude purified by silica gel column chromatography (100-200 mesh) using ethyl acetate/petrol ether (2 : 8) as eluent to get 2-(6-methyl-5-nitropyridin-2-yl)ethanol (220 mg, 55 %) as yellow liquid.

While traditionally a conservative industry, chemical producers will need to modernize their PR strategies to stay relevant.we look forward to future research findings about 15513-52-7, 2,6-Dimethyl-3-nitropyridine.

Reference:
Patent; GRUeNENTHAL GMBH; FRANK, Robert; BAHRENBERG, Gregor; CHRISTOPH, Thomas; LESCH, Bernhard; WO2013/13815; (2013); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

A new synthetic route of 2,6-Dimethyl-3-nitropyridine

With the rapid development of chemical substances, we look forward to future research findings about 15513-52-7.

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. HPLC of Formula: C7H8N2O2

A solution of 2,6-dimethyl-3-nitropyridine (50 g, 329 mmol) and SeO2 (5.02 g, 27.9 mmol) in dioxane (500 mL) was heated at reflux for 16 hours. The solution was filtered, the solvent removed and the residue purified by column chromatography directly (20% EtOAc/hexanes). The material was recrystalized from ethyl acetate to give 41 g of 6-methyl-5-nitropicolinaldehyde (41 g, 75%), a pale yellow solid; 1HNMR (CDCl3, 400 MHz) delta 2.94(s, 3H), 7.98 (d, J=8.34, 1H), 8.41 (d, J=8.34, 1H), 10.09 (s, 1H). Exact mass calculated for C7H6N2O3: 166.04, found: 167.12 MS m/z (MH+).

With the rapid development of chemical substances, we look forward to future research findings about 15513-52-7.

Reference:
Patent; Jones, Robert M.; Lehmann, Juerg; Wong, Amy Siu-Ting; Hurst, David; Shin, Young-Jun; US2006/155128; (2006); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem