Category: 556-96-7

Synthetic Route of 556-96-7, The chemical industry reduces the impact on the environment during synthesis 556-96-7, name is 1-Bromo-3,5-dimethylbenzene, I believe this compound will play a more active role in future production and life.

Copper [(I)] iodide (19 mg, 0.1 mmol), sodium iodide (300 mg, 2.0 mmol) and aryl bromide (1.2 mmol, if solid) were added to a screw-capped test tube with a Teflon-lined septum. The tube was evacuated and backfilled with argon (3 cycles). Dry toluene (1 mL), aryl bromide (1.2 mmol, if liquid) and N, N’-dimethylethylenediamine (0.2 mmol) were added by syringes at room temperature. The reaction was stirred to [110 C] for 24 hours. The reaction mixture was allowed to room temperature and the solvent was removed in [VACUO.] 2-Propanol (1.0 mL, bench top grade without degassing and pre-drying), ethylene glycol (111 [P1L,] bench top grade), aryl thiol (1.0 mmol) and potassium carbonate (276 mg, 2.0 mmol) were added at room temperature. The reaction was heated to 80 [C] and stirred for 18-20 hours. The reaction was allowed to reach room temperature. Ethyl acetate (approx. 5 mL) and dodecane (227 [PL,] GC standard) were added. The organic phase was analyzed by GC and GC-MS. The reaction was then filtered and concentrated. The crude product was purified by column chromatography on silica gel to afford the desired diaryl sulfide product. See Figure 6.

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 1-Bromo-3,5-dimethylbenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; MASSACHUSETTS INSTITUTE OF TECHNOLOGY; WO2004/13094; (2004); A2;,
Bromide – Wikipedia,
bromide – Wiktionary

Application of 556-96-7,Some common heterocyclic compound, 556-96-7, name is 1-Bromo-3,5-dimethylbenzene, molecular formula is C8H9Br, 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.

General procedure: A glassvial was charged with [Pd(IPr*me)(acac)Cl],neat amine (1.1 mmol), and the arylhalide (1 mmol) in dry 1,4-dioxane (1 mL) under an atmosphere of argonand sealed with a screw cap fitted with aseptum. LiHMDS (1.1 mmol) was subsequently injected at roomtemperature under argon, the reaction mixture was then refluxed at 110 for 3 h, After this time, dioxane was evaporated, the crude product wasdissolved in CH2Cl2. The solution was filtered on a padof silica covered with Celite, and thepad was eluted with CH2Cl2. After chromatography onsilica gel, the pure complex was obtained.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1-Bromo-3,5-dimethylbenzene, its application will become more common.

Reference:
Article; Tian, Xiabing; Lin, Jing; Zou, Sheng; Lv, Junwei; Huang, Qingfei; Zhu, Jin; Huang, Shuping; Wang, Qiwei; Journal of Organometallic Chemistry; vol. 861; (2018); p. 125 – 130;,
Bromide – Wikipedia,
bromide – Wiktionary

Reference of 556-96-7, 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 556-96-7 as follows.

General procedure: Styrene (5.0 mmol), aryl halide (5.0 mmol), potassium carbonate(10.0 mmol) and the palladium complex (0.003 mmol) weremixed in methanol (20 ml) and refluxed for 2 h as mentioned inTable 5. At the end of the reaction solvent was evaporated andthe residue was poured into water and extracted in diethyl ether,dried over anhydrous Na2SO4 and pass through 12// silica column (60-120 mesh). After evaporation of the ether, solid pure productswere obtained. The yields of the products obtained from all thereactions were determined after isolation and characterized by1H NMR spectra (Table 5).

According to the analysis of related databases, 556-96-7, the application of this compound in the production field has become more and more popular.

Reference:
Article; Das, Uttam; Pattanayak, Poulami; Patra, Debprasad; Brandao, Paula; Felix, Vitor; Chattopadhyay, Surajit; Polyhedron; vol. 110; (2016); p. 165 – 171;,
Bromide – Wikipedia,
bromide – Wiktionary

Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 556-96-7, name is 1-Bromo-3,5-dimethylbenzene, This compound has unique chemical properties. The synthetic route is as follows., Product Details of 556-96-7

General procedure: In an oven dried round bottomed flask a mixture containing styrene (2.5mmol), aryl halide (2.5mmol), the palladium complex [Pd(OL1)]4 (0.005mmol) and potassium carbonate (10.0mmol) in methanol (10cm3) was heated to reflux for 4h, as mentioned in Table 3. After the reaction was completed, the solvent was evaporated and the reaction mixture was extracted with diethyl ether. The ether solution was dried over Na2SO4 and filtered. The ether solution, containing the reaction mixture, was passed through a 12.48cm silica column (60-120 mesh), the complex was not separated out and it remained trapped in the column. After he desired compound was extracted from the column, the complex was eluted using dichloromethane. Upon evaporation of the ether, solids of the pure products were obtained. The yields of the products obtained from all the reactions were determined after isolation, and the products were characterized by 1H NMR spectra.

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 556-96-7.

Reference:
Article; Pattanayak, Poulami; Pratihar, Jahar Lal; Patra, Debprasad; Lin, Chia-Her; Chattopadhyay, Surajit; Polyhedron; vol. 63; (2013); p. 133 – 138;,
Bromide – Wikipedia,
bromide – Wiktionary

Some common heterocyclic compound, 556-96-7, name is 1-Bromo-3,5-dimethylbenzene, molecular formula is C8H9Br, 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. category: bromides-buliding-blocks

General procedure: To an oven-dried test tube equipped with a stir bar were added 0.01 mmol of Pd2(dba)3 and 0.03 mmol of ligand ((R)-Tol-BINAP or BrettPhos). Glove box was used to add 1.5 mmol ofNaOt-Pent and the tube was sealed with a Teflon screw cap. 1 mmol of aromatic halide,1.6 mmol of cyclopropylamine, and 2 mL of toluene were then added to the reaction mixture and heated at 80 C for 18 h. After completion, the reaction mixture was cooled to room temperature, diluted with diethyl ether, filtered over a short pad of silica gel, and concentrated in vacuum. Purification by flash chromatography on silica gel afforded N-cyclopropylaniline.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 556-96-7, its application will become more common.

Reference:
Article; Nguyen, Theresa H.; Maity, Soumitra; Zheng, Nan; Beilstein Journal of Organic Chemistry; vol. 10; (2014); p. 975 – 980;,
Bromide – Wikipedia,
bromide – Wiktionary

Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 556-96-7, name is 1-Bromo-3,5-dimethylbenzene, This compound has unique chemical properties. The synthetic route is as follows., Safety of 1-Bromo-3,5-dimethylbenzene

Preparation 9Preparation of (3,5-dimethyl-phenyl)-pyridin-2-yl-methanol.To a slurry of magnesium turnings (65.7 mg, 2.7 mmol) in THF (10 ml.) was added a crystal of iodine and a few drops of 1-bromo-3,5-dimethyl-benzene. The mixture was stirred at reflux temperature until the brown color started to disappear. The mixture was cooled to 0 0C, and the remaining 1-bromo-3,5-dimethyl-benzene (500 mg, 2.7 mmol) in THF was added dropwise. The reaction mixture was warmed to room temperature and was stirred until the magnesium was consumed. The reaction mixture was cooled to 0 0C, and pyridine-2-carboxaldehyde (289 mg, 2.7 mmol) in THF was added dropwise. The reaction mixture was stirred at room temperature for 30 min. The reaction was quenched with water, and the organic solution was extracted twice with ethyl acetate. The combined organic layers were washed sequentially with water and brine, and dried over MgSO4. The mixture was filtered and concentrated under reduced pressure. The residue was purified by flash chromatography (0 – 50% ethyl acetate in heptane) to afford the title compound (440 mg, 76%). 1H NMR (400 MHz, CDCI3): delta 2.29 (s, 6 H), 5.21 (br s, 1 H), 5.68 (s, 1 H), 6.91 (s, 1 H), 6.98 (br. s, 2 H), 7.16-7.21 (m, 2 H), 7.60-7.63 (m, 1 H), 8.56-8.57 (m, 1 H); MS (ES+): 214.3 (M+1 ).

According to the analysis of related databases, 556-96-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; PFIZER INC.; CAMERON, Kimberly O’Keefe; PERRY, David Austen; WO2010/67233; (2010); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Related Products of 556-96-7, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 556-96-7 name is 1-Bromo-3,5-dimethylbenzene, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

I.2 Synthesis Methods and Characterization of the CompoundsI2.1 Bis(3,5-Dimethylphenyl)Phosphinic Acid 1-Bromo-3,5-dimethylbenzene (13.63 g, 71.44 mmol, 97%) is added dropwise at room temperature to magnesium turnings (1.74 g, 71.44 mmol) in anhydrous THF (80 mL). Once the magnesium has dissolved completely, a solution of N,N-dimethylphosphoryl dichloride N(Me)2P(O)Cl2 (4.33 mL, 35.72 mmol) in anhydrous THF (10 mL) is added dropwise. To remove the salt formed in the reaction, the reaction mixture, after two hours, is added to an ice-cooled ammonium chloride solution (30 g in 500 mL of water). In a distillation apparatus, the THF is subsequently removed and the residue is boiled with concentrated HCl (75 mL) at 80 C. The resulting white solid is dissolved in aqueous NaOH (5.4 g, 300 mL of water) and the aqueous phase is extracted twice with diethyl ether. The clear aqueous phase is acidified again by adding concentrated HCl, in order to precipitate the phosphinic acid as a white solid in 70% yield (6.81 g).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1-Bromo-3,5-dimethylbenzene, and friends who are interested can also refer to it.

Reference:
Patent; BASF SE; KONINKLIJKE PHILIPS ELECTRONICS N.V.; OSRAM OPTO SEMICONDUCTORS GMBH; US2011/172423; (2011); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Related Products of 556-96-7, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 556-96-7, name is 1-Bromo-3,5-dimethylbenzene belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: CuI (0.05 mmol), aryl halide (0.5 mmol), Na3PO4 (0.5 mmol), 25-28% aqueous ammonia (1 mL), and PEG-400 (2 mL) were added to a sealed tube. The reaction mixture was stirred at 100 C (aryl iodides for 15 h and aryl bromides for 24 h) and then cooled to room temperature and extracted with diethyl ether (3 times). The combined organic phase was then dried with anhydrous Na2SO4 and the solvent was removed under reduced pressure. The remaining residue was purified by column chromatography on silica gel to provide the desired aryl amines.

The synthetic route of 1-Bromo-3,5-dimethylbenzene has been constantly updated, and we look forward to future research findings.

Reference:
Article; Chen, Junmin; Yuan, Tangjun; Hao, Wenyan; Cai, Mingzhong; Tetrahedron Letters; vol. 52; 29; (2011); p. 3710 – 3713;,
Bromide – Wikipedia,
bromide – Wiktionary

Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 556-96-7, name is 1-Bromo-3,5-dimethylbenzene, This compound has unique chemical properties. The synthetic route is as follows., Computed Properties of C8H9Br

2-bromo-3,5-dimethylbenzene 15a (1.06 g, 5.70 mmol), bis(pinacolato)diboron (2.0 g, 8.60 mmol),1,1 ‘-bis (diphenylphosphino) ferrocene] dichloropalladium (210 mg, 0.20 mmol) and potassium acetate (1.40 g, 14.30 mmol) was dissolved in 20 mL of ethylene glycol dimethyl ether and heated to reflux for 3 hours. Filtered, and the filtrate was concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography using eluent system B to give the title product, 2-(3,5-dimethylphenyl)-4,4,5,5-tetramethyl-1,3,2-dioxaborolane 15b (538 mg, yellow oil), yield: 42.1%.

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 556-96-7.

Reference:
Patent; SHANGHAI HENGRUI PHARM CO LTD; JIANGSU HENGRUI MEDICINE CO LTD; Lyu, HEJUN; DONG, QING; FEI, HONGBO; JIANG, HONGJIAN; SONG, PENG; (114 pag.)CN103030646; (2016); B;,
Bromide – Wikipedia,
bromide – Wiktionary

These common heterocyclic compound, 556-96-7, name is 1-Bromo-3,5-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. name: 1-Bromo-3,5-dimethylbenzene

Under an argon atmosphere, a solution of magnesium (25 g, 0.95 equivalent) and a small amount of iodine in THF (250 mL) was stirred at room temperature for 1 hr. 5-Bromo-m-xylene (200 g, 1.08 moL) was added at 48C, and the mixture was stirred at 5C for 1 hr. Diethyl phosphite (78.3 g, 0.52 equivalent) was added at 5C, and the mixture was stirred at 5C for 2 hrs. Water (200 mL) was added at 3C, and toluene (200 mL) and 6M-HCl (160 mL) were added. The mixture was stirred at room temperature for 30 min. The reaction mixture was partitioned, and the organic layer was washed successively with water (100 mL), 5% aqueous NaHCO3 solution (100 mL) and 5% aqueous NaCl solution (100 mL). The organic layer was dried over anhydrous magnesium sulfate and filtered by gravity. The filtrate was concentrated under reduced pressure and the residue was recrystallized from diisopropyl ether-heptane to give the title compound (43.3 g, white crystals). yield 33.3%.

The synthetic route of 1-Bromo-3,5-dimethylbenzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Takeda Chemical Industries, Ltd.; EP1452537; (2004); A1;,
Bromide – Wikipedia,
bromide – Wiktionary