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 6320-40-7 as follows. Application In Synthesis of 1,3,5-Tribromo-2-methylbenzene
Synthesis of Intermediates H and I; 2,4,6-tribromotoluene (3.3 g, 10 mmol) was dissolved in diethylether (30 ml). The reaction solution was cooled to -78 C., and n-butyllithium (4.4 ml, 11 mmol, 2.5M in hexane) was gradually added thereto. The reaction mixture was stirred at -78 C. for one hour, and copper chloride (II) (1.48 g, 11 mmol) was added thereto at -78 C. The reaction solution was stirred for five hours, and washed with distilled water and ethylacetate at room temperature. The obtained ethylacetate layer was dried over MgSO4 and then dried under a reduced pressure to obtain a crude product. The crude product was purified by silica gel column chromatography and recrystallized from dichloromethane and hexane to give intermediate H (622 mg, yield: 25%) and an intermediate I (746 mg, yield: 30%) as white solids. The structures of intermediates H and I were determined by 1H NMR. Intermediate H: 1H NMR (CDCl3, 300 MHz) delta (ppm) 7.74 (d, 4H), 7.18 (d, 4H), 2.06 (s, 6H); 13C NMR (CDCl3, 100 MHz) delta (ppm) 142.8, 134.9, 134.5, 131.1, 126.4, 119.4, 19.9. Intermediate I: 1H NMR (CDCl3, 300 MHz) delta (ppm) 7.60 (s, 4H), 2.61 (s, 6H); 13C NMR (CDCl3, 100 MHz) delta (ppm) 138.3, 137.2, 129, 9, 125.8, 23.5.
According to the analysis of related databases, 6320-40-7, the application of this compound in the production field has become more and more popular.
Reference:
Patent; Samsung SDI Co., Ltd.; US2008/174237; (2008); A1;,
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bromide – Wiktionary