Category: 75024-22-5

Related Products 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, 14.1 mmol 4-methylphenylboronic acid, 25.6 mmol sodium carbonate, 0.2 mmol tetrakistriphenylphosphine palladium, 30 ml toluene, 6 ml deionized water, and then replaced with nitrogen Three times, then 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) in a yield of 85%.Then 1.75 mmol of the obtained product, 42 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. Add hydrochloric acid to adjust the pH to 1 to precipitate largeThe white powder was collected, collected by centrifugation and dried to give a polycarboxylic acid product with a yield of 97%.Finally, 1.98 mmol of the tetracarboxylic acid product, 4 mmol of hydroxylamine hydrochloride, and 10 ml of pyridine were placed in a 50 ml single-necked flask, and heated to 90 C with an oil bath under magnetic stirring for 6 h.After the reaction, the organic solvent is depressurized under reduced pressure, then ultrasonically diluted with dilute hydrochloric acid, collected by centrifugation and dried to obtain an off-white product: an organic ligand based on NHPI functionalized polycarboxylic acid (a)The yield was 96%.

The synthetic route of 75024-22-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Tongji University; Li Liangchun; Liang Gan; Sun Chengmei; (12 pag.)CN109608381; (2019); A;,
Bromide – Wikipedia,
bromide – Wiktionary

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

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 75024-22-5, name is 1,4-Dibromo-2,3-dimethylbenzene, A new synthetic method of this compound is introduced below., Computed Properties of C8H8Br2

General procedure (a): A solution of 1,2-dimethylaryle 2b-e,h (10 mmol) and finely pulverised N-bromosuccinimide (NBS 3.68 g, 21 mmol, 2.1 equiv) in CCl4 (40-80 mL) was irradiated with HPK125 mercury lamp for 1-2 h with good stirring (tlc or 1H NMR monitoring). The reaction mixture was diluted with CH2Cl2, washed with H2O or 2 N aqueous NH4Cl solution and dried over MgSO4. The solvent was evaporated to give quantitatively 5b-e,h which was used without further purification.

The synthetic route of 75024-22-5 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Maiereanu, Carmen; Schmitt, Celine; Schifano-Faux, Nadge; Le Nouen, Didier; Defoin, Albert; Tarnus, Celine; Bioorganic and Medicinal Chemistry; vol. 19; 18; (2011); p. 5716 – 5733;,
Bromide – Wikipedia,
bromide – Wiktionary

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 75024-22-5, name is 1,4-Dibromo-2,3-dimethylbenzene, A new synthetic method of this compound is introduced below., Application In Synthesis of 1,4-Dibromo-2,3-dimethylbenzene

100 g (380 mmol) of 1,4-dibromo-2,3-dimethylbenzene are dissolved in 1500 ml of dry diethyl ether, 420 ml (840 mmol) of a 2 M solution of n-butyllithium in cyclohexane are added dropwise at -70 C., after 1 h 130 ml of trimethyl borate (1140 mmol) are added dropwise, the mixture is allowed to come to RT over the course of 1 h, the solvent is removed, 90 g (76 mmol) of pinacol and 1000 ml of toluene are added, the mixture is heated at the boil for 2 h, the solvent is removed again, and the residue, which is homogeneous according to 1H-NMR, is employed in the subsequent reaction without further purification.

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; Merck Patent GmbH; US2011/92701; (2011); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Electric Literature of 75024-22-5,Some common heterocyclic compound, 75024-22-5, name is 1,4-Dibromo-2,3-dimethylbenzene, molecular formula is C8H8Br2, 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.

Example 1 Synthesis Method of Exemplary Compound A-l Exemplary Compound A-l was synthesized according to the synthesis scheme described below.; (1) Synthesis of Intermediate 1; The following reagents and solvent were placed into a reaction vessel.1, 4-dibromo-2 , 3-dimethylbenzene : 5.00 g (18.94 mmol) N-bromosuccinimide (NBS) : 7.41 g (41.63 mmol)Anhydrous carbon tetrachloride: 100 ml[0090] Next, the mixture was stirred to dissolve the solid matters, and then the following reagent was placed into the reaction vessel.Benzoyl peroxide (BPO) : 30 mg (0.12 mmol)[0091] Next, the reaction solution was stirred for 5 hours while being heated under reflux. Next, after the reaction solution was left standing to cool, insoluble matters were filtered out, and the solvent contained in the filtrate was distilled away under reduced pressure to thereby obtain a crude product. Next, the crude product was purified by a silica gel columnchromatography (developing solvent: toluene), thereby obtaining 2.98 g (yield: 37%) of Intermediate 1.

The synthetic route of 75024-22-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; CANON KABUSHIKI KAISHA; OKAJIMA, Maki; YAMADA, Naoki; WO2011/40631; (2011); A1;,
Bromide – Wikipedia,
bromide – Wiktionary