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 460-37-7 as follows. COA of Formula: C3H4F3I
Example 447A 3-(2-Methoxypropyl)-5-methyl-2,4-dioxo-1-(3,3,3-trifluoropropyl)-1,2,3,4-tetrahydrothieno[2,3-d]pyrimidino-6-carbaldehyde (racemate) 4.33 g (13.3 mmol) of caesium carbonate were added to a solution of 2.5 g (8.86 mmol) of the compound from Ex. 442A in 18 ml of DMF, and the mixture was stirred at RT for 10 min. Then 2.98 g (13.3 mmol) of 1,1,1-trifluoro-3-iodopropane were added, and the mixture was stirred in a microwave oven (Biotage Initiator with dynamic control of irradiation power), first at 100 C. for 3 h, then at 80 C. for 3 h. After cooling to RT, about 90 ml of water were added and the product was extracted with ethyl acetate. The organic extract was washed with saturated aqueous sodium chloride solution, dried over anhydrous magnesium sulphate, filtered and concentrated. The remaining residue was purified by MPLC (Isolera, Biotage cartridge with 340 g of silica gel, cyclohexane/ethyl acetate 90:10-10:90). The product fractions were combined, concentrated by evaporation and dried under high vacuum. 2.8 g (83% of theory) of the title compound were obtained. 1H-NMR (400 MHz, DMSO-d6, delta/ppm): 10.11 (s, 1H), 4.30-4.11 (m, 2H), 4.05 (dd, 1H), 3.77 (dd, 1H), 3.63 (sext, 1H), 3.22 (s, 3H), 2.91-2.72 (m, 2H), 2.79 (s, 3H), 1.07 (d, 3H). LC/MS (Method 1, ESIpos): Rt=0.94 min, m/z=379 [M+H]+.
According to the analysis of related databases, 460-37-7, the application of this compound in the production field has become more and more popular.
Reference:
Patent; BAYER PHARMA AKTIENGESELLSCHAFT; HAeRTER, Michael; KOSEMUND, Dirk; DELBECK, Martina; KALTHOF, Bernd; WASNAIRE, Pierre; SUessMEIER, Frank; LUSTIG, Klemens; (369 pag.)US2018/65981; (2018); A1;,
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