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. COA of Formula: C3H4F3I
General procedure: Example 20A Methyl 1-(2-methoxyethyl)-3,5-dimethyl-2,4-dioxo-1,2,3,4-tetrahydrothieno[2,3-d]pyrimidine-6-carboxylate 1.246 g (3.825 mmol) of caesium carbonate were added to a solution of 402 mg (1.25 mmol) of the compound from Ex. 18A in 12.3 ml of DMF, and the mixture was stirred at RT for 10 min. Then 452 mg (3.18 mmol) of iodomethane were added, and the mixture was stirred at RT for 22 h. The reaction mixture was then partitioned between water (75 ml) and dichloromethane (75 ml). The aqueous phase was extracted with dichloromethane. The combined organic phases were dried over sodium sulphate, filtered and concentrated. The residue obtained was chromatographed on silica gel (hexane/ethyl acetate eluent). 248 mg (59% of theory) of the title compound were obtained. 1H-NMR (400 MHz, DMSO-d6, delta/ppm): 4.47 (t, 2H), 4.14-4.06 (m, 4H), 3.65 (t, 2H), 3.24 (s, 3H), 2.86-2.73 (m, 5H), 2.65-2.54 (m, 2H) LC/MS (Method 3): Rt=1.39 min, m/z=477 [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 460-37-7, 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,
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