Synthetic Route of 86604-79-7, 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 86604-79-7, name is 2,3,5-Trimethyl-4-nitropyridine 1-oxide. This compound has unique chemical properties. The synthetic route is as follows.
The 2,3,5-trimethyl-4-nitropyridine1-oxide (13.4 g, 73.6 mmol) obtained in the step (11c) was added to acetyl chloride (80 ml, 1,125 mmol) at -30 C. in a nitrogen atmosphere. The mixture was stirred at -30 C. to room temperature for 4 hours and 20 minutes. After the reaction mixture was concentrated, the residue was subjected to silica gel column chromatography (NH silica gel: 300 g, elution solvent: heptane, heptane/ethyl acetate=50/50, ethyl acetate, ethyl acetate/methanol=10/1) to obtain fractions containing a pure product of the title compound and fractions containing a crude product of the title compound. The fractions containing a crude product of the title compound was concentrated. The residue was suspended in ethyl acetate and the resulting precipitate was collected by filtration, washed with ethyl acetate and diethyl ether to obtain the title compound (Lot A, 1.58 g) as a white solid. The filtrate was concentrated. The residue was dissolved in chloroform and washed with a saturated aqueous solution of sodium hydrogen carbonate, dried over anhydrous sodium sulfate, filtered and concentrated. The residue was suspended in diethyl ether. The resulting precipitate was collected by filtration, washed with diethyl ether to obtain the title compound (Lot B, 2.69 g) as a pale brown solid. The fractions containing a pure product of the title compound were concentrated. The residue was dissolved in chloroform, washed with a saturated aqueous solution of sodium hydrogen carbonate, dried over anhydrous sodium sulfate, filtered and concentrated to obtain the title compound (Lot C, 6.56 g) as a pale white solid. The yield of the obtained title compounds of 3 lots was 85.7% in total. Lot A: 1H NMR(400 MHz, DMSO-d6) deltappm; 2.24(3H, s), 2.35(3H, s), 2.39(3H, s), 8.25(1H, s). Lot B: 1H NMR(400 MHz, DMSO-d6) deltappm; 2.24(3H, s), 2.35(3H, s), 2.39(3H, s), 8.25(1H, s). Lot C: 1H NMR(400 MHz, DMSO-d6) deltappm; 2.24(3H, s), 2.35(3H, s), 2.39(3H, s), 8.25(1H, s).
According to the analysis of related databases, 86604-79-7, the application of this compound in the production field has become more and more popular.
Reference:
Patent; Eisai Co., Ltd.; US2007/10542; (2007); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem