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. HPLC of Formula: C3H4F3I
Example 66A 3-Isobutyl-5-methyl-1-(3,3,3-trifluoropropyl)thieno[2,3-d]pyrimidine-2,4(1H,3H)-dione 3.23 g (23.39 mmol) of potassium carbonate were added to a solution of 2.23 g (9.35 mmol) of the compound from Ex. 44A in 82.6 ml of DMF, and the mixture was stirred at RT for 15 min. Then 6.48 g (28.07 mmol) of 1,1,1-trifluoro-3-iodopropane were added, and the mixture was stirred at RT for 73 h. The DMF was then very substantially distilled off and the remaining residue was partitioned between semisaturated sodium chloride solution (200 ml) and ethyl acetate (100 ml). The aqueous phase was extracted with ethyl acetate. The combined organic phases were dried over sodium sulphate, filtered and concentrated. The residue obtained was chromatographed using a silica gel cartridge (Biotage, 340 g of silica gel, eluent: hexane/ethyl acetate). In this way, 2.67 g (84% of theory) of the title compound were obtained. 1H-NMR (400 MHz, DMSO-d6, delta/ppm): 6.88 (d, 1H), 4.13 (t, 2H), 3.71 (d, 2H), 2.84-2.70 (m, 2H), 2.38 (d, 3H), 2.11-1.96 (m, 1H), 0.85 (d, 6H). LC/MS (Method 3): Rt=1.4 min, m/z=335 [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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