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 1003-68-5 as follows., 1003-68-5
To 144 5-methyl-1H-pyridin-2-one (2.0 g, 18 mmol), 96 1-iodo-4-(trifluoromethyl)benzene (5.9 g, 22 mmol), 12 copper(I) iodide (6.7 g, 3.6 mmol), 13 potassium phosphate (7.7 g, 37 mmol) and 145 N,N’-dimethylethylenediamine (0.70 g, 7.3 mmol) was added 126 1,4-dioxane (15 mL), and the mixture was stirred under a nitrogen atmosphere at 109C overnight. Insoluble material was filtered off through celite, the filtrate was poured into water and the mixture was extracted three times with ethyl acetate. The organic layer was dried over sodium sulfate. The desiccant was filtered off, and the filtrate was concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (petroleum ether/ethyl acetate) to give the 146 title compound (4.2 g, 17 mmol, 91%). 1H NMR (400 MHz, DMSO-d6) delta7.90 (d, J = 8.0 Hz, 2H), 7.68 (d, J = 8.4, Hz, 2H), 7.52 (s, 1H) 7.41 (dd, J = 2.8, 9.6 Hz, 1H), 6.48 (d, J = 9.2 Hz, 1H) 2.05 (s, 3H).
The chemical industry reduces the impact on the environment during synthesis 1003-68-5, I believe this compound will play a more active role in future production and life.
Reference:
Patent; EA Pharma Co., Ltd.; KOBAYASHI, Kaori; SUZUKI, Tamotsu; OKUZUMI, Tatsuya; (110 pag.)EP3412664; (2018); A1;,
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