Electric Literature of 26670-89-3,Some common heterocyclic compound, 26670-89-3, name is 2-Bromo-4-iodo-1-methylbenzene, molecular formula is C7H6BrI, 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.
In a 1 L four-necked round bottom flask equipped with a stirrer, Erlin condenser, nitrogen inlet tube, and thermometer, 19.3 g (91.0 mmol) of 4-dibenzofuran boronic acid of Synthesis Example 8, 2 (100.0 mmol) of bromo-4-iodotoluene, 300 mL of toluene, 150 mL of ethanol, 25.1 g (181.5 mmol) of potassium carbonate and 90 mL of water, and the mixture was stirred at room temperature for 30 minutes under a nitrogen stream. Subsequently, 0.10 g (0.45 mmol) of palladium acetate and 0.27 g (0.91 mmol) of tri (o-tolyl) phosphine were added and heated, followed by stirring at a reflux temperature for 2 hours. The resulting reaction solution was cooled to room temperature, the aqueous layer was separated, and extracted twice with 100 mL of ethyl acetate. Next, the organic layers were combined, washed with 100 mL of saturated brine, dried over magnesium sulfate, magnesium sulfate was removed by suction filtration, and the solvent was distilled off under reduced pressure. Subsequently, the obtained oily matter was separated by silica gel column chromatography with a mixed solvent of n-heptane and toluene to obtain 23.3 g (yield: 75.9%) of the desired bromide.
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2-Bromo-4-iodo-1-methylbenzene, its application will become more common.