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 202982-67-0 as follows. name: 4-Chloro-3-fluoroiodobenzene
Tris(dibenzylideneacetone)dipalladium(0) (47.6 mg, 0.05 mmol), 2- (dicyclohexylphosphino)-2′,4′,6′-triisopropylbiphenyl (XPhos, 49.6 mg, 0.10 mmol), 4-chloro-3- fluoroiodobenzene (400 mg, 1.56 mmol, Aldrich), teri-butyl 2,6-diazaspiro[3.3]heptane-2- carboxylate, oxalic acid (300 mg, 1.04 mmol, ArkPharm), and cesium carbonate (1017 mg, 3.12 mmol) were suspended in dioxane (12 mL). The reaction mixture was stirred at 98 C for 18 hours and then cooled to ambient temperature. The crude reaction mixture was combined with 5 grams of Celite and concentrated under reduced pressure to a free flowing powder. The powder was directly purified by reversed-phase flash chromatography [Interchim PuriFlash C18XS 30 mupiiota 175 g column, flow rate 100 mL/minute, 5-100% gradient of acetonitrile in buffer (0.025 M aqueous ammonium bicarbonate, adjusted to pH 10 with ammonium hydroxide)] to give the title compound (0.27 g, 0.83 mmol, 79 % yield).JH NMR (400 MHz, DMSO-de) delta ppm 7.29 (t, J = 8.6 Hz, 1H), 6.42 (dd, J = 11.7, 2.6 Hz, 1H), 6.25 (ddd, J = 8.8, 2.6, 0.8 Hz, 1H), 4.01 (s, 4H), 3.94 (s, 4H), 1.38 (s, 9H); MS (ESI+) m/z 327 (M+H)+.
According to the analysis of related databases, 202982-67-0, the application of this compound in the production field has become more and more popular.
Reference:
Patent; CALICO LIFE SCIENCES LLC; ABBVIE INC.; MARTIN, Kathleen Ann; SIDRAUSKI, Carmela; FROST, Jennifer M.; TONG, Yunsong; XU, Xiangdong; SHI, Lei; XIONG, Zhaoming; (165 pag.)WO2019/90090; (2019); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com