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 19393-94-3 as follows. Quality Control of 2,4-Dibromo-1-iodobenzene
Synthesis of Intermediate A2; Intermediate A1 (2.5 g, 6.9 mmoles), 1-pyreneboronic acid (1.7 g, 6.9 mmoles) and tetrakis(triphenylphosphine)palladium(0) (0.24 g, 0.21 mmoles, 3% Pd) were suspended in 1,2-dimethoxyethane (20 mL) under a nitrogen atmosphere, to which was then added a 2M sodium carbonate aqueous solution (2.2 g, 21 mmoles, 3 eq./10 mL), and the mixture was refluxed for 10 hours. Toluene (150 mL) and water (50 mL) were added to the reaction mixture, an organic layer was aliquoted, washed with saturated salt water (50 mL) and then dried over anhydrous magnesium sulfate, and the solvent was distilled off to obtain a pale yellow solid. This was purified by means of column chromatography (silica gel/hexane and 17% dichloromethane) to obtain a white solid (1.9 g, 63%). 1H-NMR (400 MHz, CDCl3, TMS): delta7.32 (1H, d, J = 8 Hz), 7.60 (1H, dd, J = 8 Hz, 2 Hz), 7.68 (1H, d, J = 9 Hz), 7.83 (1H, d, J = 8 Hz), 7.96 to 8.02 (3H, m), 8. 10 (2H, s), 8.16 (1H, d, J = 8 Hz), 8.20 (1H, d, J = 8 Hz), 8.21 (1H, d, J = 8 Hz)
According to the analysis of related databases, 19393-94-3, the application of this compound in the production field has become more and more popular.
Reference:
Patent; Idemitsu Kosan Co., Ltd.; EP2316816; (2011); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com