Synthetic Route of 52548-63-7, 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 52548-63-7 as follows.
To a 500 mL round- bottomed flask was added 5-fluoro-2-iodo-benzoic acid (23 g, 86.5 mmol) in methanol (230 mL). To the resulting solution was added cone, sulfuric acid (2.3 mL, 43.2 mmol). The reaction mixture was warmed to 65 oC and stirred for 15 h. The resulting mixture was concentrated under reduced pressure to give crude producte which was then was partitioned between EtOAc (250 mL) and a half sat. Na2CO3(ac?) solution (250 mL). The layers were thoroughly mixed and then separated. The organic layer was dried over magnesium sulfate, filtered, and concentrated under reduced pressure to give a yellow oil (23 g, 95% yield). 1 H NMR (400 MHz, CDCI3): 7.94 (dd, J = 8.7, 5.4 Hz, 1 H), 7.54 (dd, J = 9.0, 3.1 Hz, 1 H), 6.93 (m, 1 H), 3.94 (s, 3H).
According to the analysis of related databases, 52548-63-7, the application of this compound in the production field has become more and more popular.
Reference:
Patent; JANSSEN PHARMACEUTICA NV; CHAI, Wenying; LETAVIC, Michael, A.; LY, Kiev, S.; PIPPEL, Daniel, J.; RUDOLPH, Dale, A.; SAPPEY, Kathleen, C.; SAVALL, Brad, M.; SHAH, Chandravadan, R.; SHIREMAN, Brock, T.; SOYODE-JOHNSON, Akinola; STOCKING, Emily, M.; SWANSON, Devin, M.; WO2011/50198; (2011); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com