Electric Literature of 116632-39-4, A common heterocyclic compound, 116632-39-4, name is 5-Bromo-2-iodotoluene, molecular formula is C7H6BrI, its 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.
Synthesis of Raw Material Compound 6 4-Benzoylphenylboronic acid (6.25 g) (21 mmol), 5.23 g of 5-bromo-2 iodotoluene (23 mmol), and 6.68 g of sodium carbonate (63 mmol) are dissolved in 130 ml of ethylene glycol dimethyl ether-distilled water mixed solvent (10:3), and then 0.24 g of palladium acetate (1.05 mmol) and 0.55 g of triphenylphosphine (2.1 mmol) are added thereto, and the reaction system is subjected to heating for 3 hour under nitrogen flow.After the reaction solution is allowed to be cooled, distilled water and about 600 ml of ethyl acetate are added and extraction is performed. After removing an aqueous layer and separating an organic layer, the system is dried with magnesium sulfate. The filtrate from which magnesium sulfate is filtered out is evaporated to dryness in a rotary evaporator, and refined by silica gel column (ethyl acetate: hexane=1:40?1:10) to obtain 6.6 g of white to pale yellow raw material compound 6 (yield: 90%). The obtained compound 6 is confirmed to be an objective compound by mass spectrum and 1H NMR spectrum.
The synthetic route of 116632-39-4 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; FUJIFILM CORPORATION; US2012/319059; (2012); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com