Some common heterocyclic compound, 5469-19-2, name is 1-Bromo-2,4,5-trimethylbenzene, molecular formula is C9H11Br, 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. Safety of 1-Bromo-2,4,5-trimethylbenzene
d. N,N’-(4,4′-(cyclohexane-1 ,1 -diyl)bis(4, 1 -phenylene))bis(2,4,5-trimethyl- N-(2,4,5-trimethylphenyl)aniline) In a dry box, 4,4′-(cyclohexane-1 , 1 -diyl)dianiline (6.75 g, 25.09 mmol), 1 – bromo-2,4,5-trimethylbenzene (21 .19 g, 105.36 mmol), tris(tert- butyl)phosphine (0.41 g, 2.01 mmol) and Pd2(DBA)3 (0.92 g, 1 .00 mmol) were combined in round bottom flask and dissolved in 450 ml of dry toluene. The solution was stirred for a minute and followed by sodium tert- butoxide (10.61 g, 1 10.38 mmol) and 50 ml of dry toluene. A heating mantle was added and the reaction heated to 80C for 18 hour. The reaction mixture was then cooled to room temperature and filtered, washing with chloroform. The solvent was removed by rotary evaporation and the residue was purified further by silica gel column chromatography using a gradient of chloroform in hexanes (0-25%). The product containing fractions were collected and combined. The solvent was removed by rotary evaporation. The crude product was dissolved in DCM (100 ml_) and precipitated into methanol (700 ml_) to give 1 7.47 g (94%) product as a white powder. 1 H NMR (CDCI3) is consistent with structure.
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 5469-19-2, its application will become more common.
Reference:
Patent; E. I. DU PONT DE NEMOURS AND COMPANY; WANG, Ying; WU, Weishi; DOBBS, Kerwin, D.; WO2011/49904; (2011); A2;,
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