Reference of 75024-22-5, These common heterocyclic compound, 75024-22-5, name is 1,4-Dibromo-2,3-dimethylbenzene, 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.
Add 6.3 mmol to a 100 ml three-necked flask under N2 protection.1,4-Dibromo-2,3-dimethylbenzene, 13.5 mmol 3,5-dimethylphenylboronic acid25.6mmol potassium carbonate, 0.2mmol tetrakistriphenylphosphine palladium,30 ml of 1,4-dioxane, 6 ml of deionized water, and then replaced with nitrogen three times.Then, it was heated to 90 C with an oil bath under magnetic stirring for 6 h. After the reaction,After washing with water, extracting, drying, and removing the organic solvent under reduced pressure,The product was isolated by column chromatography (petroleum ether), yield 88%.1.9 mmol of the obtained product, 68 mmol of potassium permanganate, 10 ml of pyridine,12 ml of distilled water was added to a 100 ml three-necked flask, and then heated to 100 C with an oil bath under magnetic stirring, and the reaction was refluxed for 15 hours. After the reaction was completed, the organic solvent was depressurized under reduced pressure, and then water was added thereto. After ultrasonic etching, MnO 2 was filtered through celite.Adding hydrochloric acid to adjust the pH to 1 can precipitate a large amount of white powder, collect by centrifugation and dry.The polycarboxylic acid product was obtained in a yield of 94%.Finally, 1.8 mmol of hexacarboxylic acid product, 4 mmol of hydroxylamine hydrochloride,10 ml of pyridine was added to a 50 ml single-necked flask and heated to 90 C with an oil bath under magnetic stirring.Reaction for 6 h. After the reaction, the organic solvent was depressurized under reduced pressure, and then diluted with hydrochloric acid for a while, collected by centrifugation and dried to obtain an off-white product b with a yield of 97%.
Statistics shows that 1,4-Dibromo-2,3-dimethylbenzene is playing an increasingly important role. we look forward to future research findings about 75024-22-5.
Reference:
Patent; Tongji University; Li Liangchun; Liang Gan; Sun Chengmei; (12 pag.)CN109608381; (2019); A;,
Bromide – Wikipedia,
bromide – Wiktionary