Some common heterocyclic compound, 24988-36-1, name is 1,5-Dibromo-2,4-dimethoxybenzene, molecular formula is C8H8Br2O2, 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. Computed Properties of C8H8Br2O2
Add to the dry three-necked flask with a magnetic rotor 1,3-dibromo-4,6-dimethoxybenzene (3.0515 g, 10 mmol, 97%, 1.0 eq),4-biphenylboronic acid (4.4449 g, 22 mmol, 98%, 2.2 equivalents),palladium acetate (0.0674g, 0.3mmol,0.03 equivalents) and the ligand S-Phos (0.2513 g, 0.6 mmol, 98%, 0.06 equivalents).Nitrogen gas was distilled off three times, and then an aqueous solution (20 mL) of 1,4-dioxane (60 mL) and potassium carbonate (6.9100 g, 50 mmol, 5.0 eq. The three vials were then placed in a 110 C oil bath. After stirring for 24 hours, the reaction was monitored by thin layer chromatography. After cooling to room temperature, the organic phase was separated and aqueous was extracted with ethyl acetate (30mL×2).The organic phases were combined, dried over anhydrous sodium sulfate, filtered and evaporated.The crude product was separated and purified by flash column chromatography on silica gel (eluent: petroleum ether / ethyl acetate = 50/1) to give A5, white solid 4.4216g, 99% yield.
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 24988-36-1, its application will become more common.
Reference:
Patent; Zhejiang University of Technology; Li Guijie; Dai Jianxin; Chen Shaohai; Feng Qi; (28 pag.)CN110183476; (2019); A;,
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