At the same time, in my other blogs, there are other synthetic methods of this type of compound, 118431-88-2, and friends who are interested can also refer to it.
118431-88-2, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 118431-88-2 as follows.
[Example 4]; Production of 2-cyano-3-cyclopropyl-1-[1,2-dihydro-1-methyl-2-oxo-6-(trifluoromethyl)pyridin-3-yl]propane-1,3-dione (Inventive Compound No. V-9); 1,2-dihydro-1-methyl-2-oxo-6-(trifluoromethyl)pyridine-3-carboxylic acid (1.0g, 4.5 mmol) was dissolved in thionyl chloride (5 mL), and the mixture was refluxed for 2 hours. The reaction solution was concentrated under reduced pressure to obtain 1,2-dihydro-1-methyl-2-oxo-6-(trifluoromethyl)pyridine-3-carbonyl chloride. The obtained acid chloride was dissolved in acetonitrile (20 mL), and added dropwise to a mixed solution of 3-cyclopropyl-3-oxopropanenitrile (0.49g, 4.5 mmol), triethylamine (0.55g, 5.4 mmol) and acetonitrile (10 mL), under ice cooling. After the stirring for a day at room temperature, acetonecyanhydrin (0.04g, 0.47 mmol) and triethylamine (0.55g, 5.4 mmol) were further added thereto, and the mixture was stirred for a day at room temperature. The reaction mixture was concentrated under reduced pressure, and thus obtained residue was added with a mixture of aqueous saturated sodium bicarbonate and ethyl acetate for liquid separation. The obtained aqueous layer was added with diluted hydrochloric acid to give a pH of 3 to 4, and extracted with chloroform. The obtained organic layer was dried over anhydrous magnesium sulfate, the solvent was distilled off under reduced pressure, and thus obtained crystal was washed with ether, to obtain 0.29g of a subject compound (yield: 20%). 1H-NMR Data (CDCl3/TMS delta (ppm)): 1.24-1.31 (2H, m), 1.39-1.44 (2H, m), 2.35-2.43 (1H, m), 3.71 (3H, d), 6.77 (1H, d, J=7.4 Hz), 7.72 (1H, d, J=7.4 Hz), 17.2 (1H, s)
At the same time, in my other blogs, there are other synthetic methods of this type of compound, 118431-88-2, and friends who are interested can also refer to it.
Reference:
Patent; KUMIAI CHEMICAL INDUSTRY CO., LTD.; IHARA CHEMICAL INDUSTRY CO., LTD.; EP1982978; (2008); A1;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts