Reference of 63262-06-6, A common heterocyclic compound, 63262-06-6, name is 1,4-Dibromo-2,5-diiodobenzene, molecular formula is C6H2Br2I2, 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.
A nitrogen gas atmosphere was prepared in a reaction vessel equipped with a stirrer, then, a compound 1 (22.0 g), 2-bromophenylboronic acid (19.1 g), tetrakis(triphenylphosphine)palladium(0) (2.43 g) and tetrahydrofuran (440 mL) were added, and the mixture was heated at 45 C. Thereafier, to this was added silver carbonate (47.2 g), and the mixture was refluxed for 3 hours. The resultant reaction liquid was cooled down to room temperature, then, water and toluene were added, and the mixture was stirred at room temperature. Thereafter, the aqueous layer was separated, and the organic layer was washed with a saturated sodium chloride aqueous solution. To the resultant organic layer was added sodium sulfate, then, the layer was filtrated, and concentrated to obtain a coarse product. Thereafier, to this were added toluene and activated carbon, and the mixture was stirred at 70 C. for 1 hour. Thereafter, the mixture was filtrated through a filter pre-coated with Celite. The resultant residue was washed with toluene several times. The resultant washing liquid was concentrated, then, recrystallized using toluene, thereby obtaining 17.9 g of a compound 2 (yield:74%, purity: 98.9%) as a white solid. ?H-NMR (DMSO-d5, 300 MHz): oe (ppm)7.43 (4H, t), 7.49 (2H, t), 7.71 (2H, d), 7.76 (2H, d).
The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.
Reference:
Patent; Sumitomo Chemical Company, Limited; USUI, Motoaki; FUKUSHIMA, Daisuke; TANAKA, Shin-ya; (58 pag.)US2017/137566; (2017); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com