Category: 74137-36-3

Adding a certain compound to certain chemical reactions, such as: 74137-36-3, name is 1,3-Dibromo-5-methoxybenzene, belongs to ethers-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 74137-36-3, Recommanded Product: 74137-36-3

To a solution of 1,3-dibromo-5-methoxybenzene (9.18 mmol, 1 eq) in 2 ml of xylene under a nitrogen atmosphere, acrylic acid (0.63 ml, 9.18 mmol, 1 eq), Pd(OAc)2 (1 mole percent, 20.66 mg), triphenylphosphine (4 mole percent, 69.2 mg) and triethylamine (19.278 ml, 2.7, 2.1 eq) are added. The reaction mixture is stirred at 100° C. for 11 h. Thereafter, 20 ml of water and 2 g of sodium carbonate were added, and the mixture was stirred at 100° C. for some minutes. The aqueous phase was subsequently separated and acidified. The precipitate that formed was dried and purified by means of column chromatography (eluent hexane/ethyl acetate 1/1) to obtain the desired product in a yield of 32percent (751 mg). C10H9Br3O; MW 256/258; 1H-NMR (CD3OD): delta 7.61 (d, J=16.1 Hz, 1H), 7.38-7.37 (m, 1H), 7.17-7.16 (m, 2H), 6.53 (d, J=16.1 Hz, 1H), 3.87 (s, 3H); 13C-NMR (CD3OD): delta 169.8, 162.3, 144.5, 138.9, 124.2, 121.4, 120.0, 113.4, 56.2

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, 1,3-Dibromo-5-methoxybenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Hartmann, Rolf; Frotscher, Martin; Oberwinkler, Sandrine; Ziegler, Erika; Messinger, Josef; Thole, Heinrich-Hubert; US2010/204234; (2010); A1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

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. 74137-36-3, name is 1,3-Dibromo-5-methoxybenzene, A new synthetic method of this compound is introduced below., Recommanded Product: 1,3-Dibromo-5-methoxybenzene

A mixture of 3,5-dibromoanisole (10 mmol, 2.7 g)Diphenylamine (60 mmol, 10 g) was added to a 100 mL three-necked flask,A cuprous iodide (6 mmol, 1.2 g) was added under nitrogen,Potassium carbonate (60 mmol, 8.3 g),Phenanthroline (6 mmol, 1.2 g),50 mL of DMF,The reaction was carried out at 155 ° C for 3 days;The resulting reaction product is subjected to extraction,The extracted organic phase was evaporated to dryness with ethanol,Then recrystallized from ethyl acetate and petroleum ether,To give 4.02 g of intermediate C-1,

The synthetic route of 74137-36-3 has been constantly updated, and we look forward to future research findings.

Adding a certain compound to certain chemical reactions, such as: 74137-36-3, name is 1,3-Dibromo-5-methoxybenzene, belongs to ethers-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 74137-36-3, Product Details of 74137-36-3

The Bl (3.34g, 10 mmol) was added vial, the injection of THF dried, placed in a dry ice – acetone bath cooling, -78 ° C was added dropwise n-BuLi (1 lmmol, 2.5M) solution, stirring was continued for 3 hours and then triisopropyl borate (2.07g, 11 mmol) added to the bottle, slowly brought to room temperature and stirred overnight. After completion of the reaction, dilute HC1 solution was dropwise jerk, and extracted with methylene chloride, the organic layer was dried, solvent was removed, dichloromethane and petroleum ether (60-90) was washed with a mixture of beating to give D-1 (2.57g, y = 86percent),

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

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. 74137-36-3, name is 1,3-Dibromo-5-methoxybenzene, A new synthetic method of this compound is introduced below., Formula: C7H6Br2O

The mixture of 1,3-dibromo-5-methoxybenzene (0.5 g,1.88 mmol), bis(pinacolato)diboron (1.05 g, 4.1 mmol), PdCl2(dppf)(140 mg, 0.23 mmol), potassium acetate (1.1 g,11.3 mmol), and DMF(40 mL) were stirred for 2.5 h at 80 C. The solvent was removed invacuo and the residue was dissolved in CH2Cl2. The solution waswashed with water and dried over magnesium sulfate. The filtratewas concentrated to dryness, and the residue was purified by flashcolumn chromatography on silica gel (eluent: petroleum ether/CH2Cl2 = 10/1), gave compound 3 as a white solid. Yield: 383 mg(56%). 1H NMR (400 MHz, CDCl3) delta (ppm): 7.87 (s, 1H), 7.42 (d,J 0.9 Hz, 2H), 3.84 (s, 3H), 1.33 (s, 24H). 13C NMR (100 MHz, CDCl3) delta (ppm): 158.56, 133.60, 122.79, 83.78, 55.33, 24.87. MS (EI): m/z 359.9.

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.

Electric Literature of 74137-36-3, These common heterocyclic compound, 74137-36-3, name is 1,3-Dibromo-5-methoxybenzene, 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.

To a solution of 20b (60 g, 0.2256 mol) and anhydrous Et2O (1 L)cooled to -78¡ã C. and maintained under an Ar atmosphere was added dropwise over 30 min n-BuLi (100 mL, 0.2482 mol, 2.5M in hexane). The yellow solution was stirred at -78¡ã C. for 20 min. To the reaction mixture was added dropwise dry DMF (19 mL, 248.2 mmol) over 15 min and the reaction stirred at -78¡ã C. for 10 min before the cooling bath was removed and the reaction allowed to warm to -30¡ã C. over 30 min. The reaction vessel was placed in an ice-water bath and warmed to -10¡ã C. The mixture was slowly added to an ice cold saturated aqueous NH4Cl solution (400 mL). The organic layer was separated and the aqueous phase thrice extracted with Et2O. The combined extracts were washed with water, dried (MgSO4), filtered and evaporated to afford an oil which solidified on standing. The crude product was purified by SiO2 chromatography eluting with a hexane/EtOAc gradient (3 to 5percent EtOAc) to afford 21.

The synthetic route of 74137-36-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Roche Palo Alto LLC; US2007/88015; (2007); A1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Related Products of 74137-36-3, 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. 74137-36-3, name is 1,3-Dibromo-5-methoxybenzene, This compound has unique chemical properties. The synthetic route is as follows.

Step 3: Pd(PPh3)4 (600 mg, 0.53 mmol, 0.1 eq.) and Cs2CO3 (3.40 g,10.52 mmol, 2.0 eq.) were added to a stirred solution of N-(5-(4,4,5,5- tetramethyl-1 ,3,2-d ioxaborolan-2-yl)-pyridi n-2-yl)-2-methylpyri midi ne-5-carboxamide (1 .78 g, 5.26 mmol, 1 .0 eq.) and dibromoanisole (1 .40 g, 5.26 mmol, 1.0 eq.) in dioxane (14 ml) at RT under a nitrogen atmosphere. The reaction mixture was heated to 100 ¡ãC for 16 h after which time it was allowed to cool to RT. The reaction mixture was then filtered and the filtrate was concentrated under reduced pressure. The residue was diluted withethyl acetate (100 mL) and washed with water and brine (100 mL each). The organic layer was dried over Na2504 and concentrated under reduced pressure to give crude product. This material was purified by flash chromatography (over silica gel 230-400 mesh) eluting with 2 percent methanol in DCM to afford pure N-[5-(3-bromo-5-methoxyphenyl)pyridin-2-yl]-2-methylpyrimidine-5-carboxamide (1.20 g; 57percent).

The chemical industry reduces the impact on the environment during synthesis 1,3-Dibromo-5-methoxybenzene. I believe this compound will play a more active role in future production and life.

Reference:
Patent; FROST BIOLOGIC, INC.; SIDDIQUI-JAIN, Adam; WO2015/127284; (2015); A2;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Application of 74137-36-3,Some common heterocyclic compound, 74137-36-3, name is 1,3-Dibromo-5-methoxybenzene, molecular formula is C7H6Br2O, 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.

To a 250 mL two-necked flask was added 3,5-dibromoanisole (9) (5 g, 18.8 mmol, 1 eq.) Under argon, Anhydrous CH2Cl2 (80 mL) was added, BBr3 (3.5 mL, 37.6 mmol, 2 eq.) Was added dropwise at 0 ¡ã C and maintained at 0 ¡ã C for 3 hours and then allowed to warm to room temperature, The reaction was stopped after darkening for 2 days. The reaction was extracted with CH2Cl2 (50 mL x 3) Combine organic phase, Distilled water (50 mL x 3), Dried over anhydrous magnesium sulfate, The magnesium sulfate was removed by filtration, Steaming the solvent, The residue was purified by silica gel column chromatography (eluent: ether / petroleum ether = 1/9) 4.2 g of a white solid, Yield 90percent. Mp = 86-89 ¡ã C.

The synthetic route of 74137-36-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Donghua University; Jin, Wusong; Zhang, Dengqing; Xiao, Duoduo; Li, Xianying; Chen, Beihua; Ning, Ruguang; Zhang, Zhen; (13 pag.)CN103819479; (2017); B;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

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 74137-36-3 as follows. Safety of 1,3-Dibromo-5-methoxybenzene

Tris (dibenzylideneacetone) [DIPALLADIUM (0)] (6.53g, 7. [15MMOL)] was added in one portion to a stirred solution of the bromide of Preparation 1 (38. 0g, [143MMOL),] 1,1′-bis (diphenylphosphino) ferrocene (9.3g, 16. [8MMOL)] and zinc cyanide (20. 0g, [172MOL)] in N,N-dimethylformamide (300ml) at room temperature under nitrogen. The reaction was heated at [100¡ãC] for 14 hours and cooled to room temperature. Water (1500ml) was added and the mixture was extracted with ethyl acetate [(3X500ML).] The combined organics were filtered and the filtrate was washed with water (500ml), dried over magnesium sulphate, filtered and concentrated under reduced pressure. The resulting solid was triturated with toluene (1000ml) to provide the title compound (18. 0g) as a tan solid.

According to the analysis of related databases, 74137-36-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Pfizer Limited; Pfizer Inc.; WO2004/31156; (2004); A1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Adding a certain compound to certain chemical reactions, such as: 74137-36-3, name is 1,3-Dibromo-5-methoxybenzene, belongs to ethers-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 74137-36-3, category: ethers-buliding-blocks

Tris (dibenzylideneacetone) [DIPALLADIUM (0)] (6.53g, 7. [15MMOL)] was added in one portion to a stirred solution of the bromide of Preparation 1 (38. [0G,] [143MMOL),] 1,1′-bis (diphenylphosphino) ferrocene (9.3g, 16. [8MMOL)] and zinc cyanide (20. 0g, [172MMOL)] in [NN-DIMETHYLFORMAMIDE (300ML)] at room temperature under nitrogen. The reaction was heated at [100¡ãC] for 14 hours and cooled to room temperature. Water [(1500ML)] was added and the mixture was extracted with ethyl acetate [(3X500M1).] The combined organics were filtered and the filtrate was washed with water [(500MOI),] dried over magnesium sulphate, filtered and concentrated under reduced pressure. The resulting solid was triturated with toluene [(1000MOL)] to provide the [TITLE COMPOUND (1 8. 0G)] as a tan solid. [1H-NMR] [(300MHZ,] [CDC13)] : [8] = 3.83 (3H, s), 7.31 (2H, s), 7.48 [(1 H,] s).

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

Reference:
Patent; PFIZER LIMITED; PFIZER INC.; WO2004/29051; (2004); A1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Reference of 74137-36-3, These common heterocyclic compound, 74137-36-3, name is 1,3-Dibromo-5-methoxybenzene, 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.

step 2-To a solution of R-27b (60 g, 0.2256 mol) and anhydrous Et2O (1 L) cooled to -78 C. and maintained under an Ar atmosphere was added dropwise over 30 min n-BuLi (100 mL, 0.2482 mol, 2.5M in hexane). The yellow solution was stirred at -78 C. for 20 min. To the reaction mixture was added dropwise dry DMF (19 mL, 248.2 mmol) over 15 min and the reaction stirred at -78 C. for 10 min before the cooling bath was removed and the reaction allowed to warm to -30 C. over 30 min. The reaction vessel was placed in an ice-water bath and warmed to -10 C. The mixture was slowly added to an ice cold saturated aqueous NH4Cl solution (400 mL). The organic layer was separated and the aqueous phase thrice extracted with Et2O. The combined extracts were washed with water, dried (MgSO4), filtered and evaporated to afford an oil which solidified on standing. The crude product was purified by SiO2 chromatography eluting with a hexane/EtOAc gradient (3 to 5% EtOAc) to afford R-28.

The synthetic route of 74137-36-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Billedeau, Roland Joseph; Sweeney, Zachary Kevin; US2009/170856; (2009); A1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem