A common heterocyclic compound, 1646-54-4, name is 1,4-Dibromo-2,3,5,6-tetramethylbenzene, molecular formula is C10H12Br2, 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. 1646-54-4.
The reaction pathway is shown in Scheme 1. H4dbtec ligand was prepared according literature [13] and with a little modification. To a four-necked flask equipped with a reflux condenser and a mechanical stirrer, 3,6-bromo-tetramethylbenzene (0.171 mol), 2.1 L pyridine and 280 mL water were added. The reaction mixture was heated to 100 C while stirring. KMnO4 (0.859 mol) was added in small portions and the mixture was refluxed for 5 h. The warm solution was separated from MnO2 by filtration and the solvent evaporated under reduced pressure. 280 mL water and 112 g NaOH were added to the residual solid. After the combined mixture was heated up to 100 C, KMnO4 (0.859 mol) was added again in small portions and the mixture was refluxed for 5 h. The excess KMnO4 was destroyed by the cautious addition of 140 mL ethanol. The MnO2 was removed from the hot mixture by filtration. The filtrate was acidified with aqueous HCl (5 M, 600 mL). After the solvent was revaporated, the residue was washed with acetone. The resultant solid was dried. The yield was 46 g (66%). 1H NMR (300 MHz; DMSO-d6) no signals. 13C NMR (100 MHz; DMSO-d6) deltac 115.51, 137.57, 166.27.
The synthetic route of 1,4-Dibromo-2,3,5,6-tetramethylbenzene has been constantly updated, and we look forward to future research findings.
Reference:
Article; Zhang, Liang-Liang; Guo, Yu; Wei, Yan-Hui; Guo, Jie; Wang, Xing-Po; Sun, Dao-Feng; Journal of Molecular Structure; vol. 1038; (2013); p. 73 – 77;,
Bromide – Wikipedia,
bromide – Wiktionary