Related Products of 460-37-7,Some common heterocyclic compound, 460-37-7, name is 1,1,1-Trifluoro-3-iodopropane, molecular formula is C3H4F3I, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
Example 168A Ethyl 3-ethyl-2,4-dioxo-5-(trifluoromethyl)-1-(3,3,3-trifluoro9propyl)-1,2,3,4-tetrahydrothieno[2,3-d]pyrimidine-6-carboxylate 1.39 g (13.1 mmol) of caesium carbonate were added to a solution of 2.0 g (5.95 mmol) of the compound from Ex. 165A in 40 ml of DMF, and the mixture was stirred at RT for 15 min. Then 2.66 g (11.9 mmol) of 3,3,3-trifluoro-1-iodopropane were added, and the mixture was heated at 60 C. After 1 h, a further 2.66 g (11.9 mmol) of 3,3,3-trifluoro-1-iodopropane were added. Stirring at 60 C. was continued for 16 h. After cooling to RT, about 160 ml of water were added and the mixture was extracted three times with about 80 ml of diethyl ether each time. The combined organic extracts were washed with saturated sodium chloride solution. After drying over anhydrous magnesium sulphate, the mixture was filtered and the filtrate was evaporated. The crude product was purified by MPLC on a Puriflash cartridge (100 g of silica gel, cyclohexane/ethyl acetate 7:1?1:1). The product fractions were combined and concentrated, and the residue was dried under high vacuum. 1.86 g (72% of theory) of the title compound were obtained. 1H-NMR (400 MHz, CDCl3, delta/ppm): 4.41 (q, 2H), 4.20 (t, 2H), 4.08 (q, 2H), 2.73-2.61 (m, 2H), 1.40 (t, 3H), 1.26 (t, 3H). LC/MS (Method 1, ESIpos): Rt=1.15 min, m/z=433 [M+H]+.
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1,1,1-Trifluoro-3-iodopropane, its application will become more common.
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;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com