Category: 138526-69-9

Adding a certain compound to certain chemical reactions, such as: 138526-69-9, name is 1-Bromo-3,4,5-trifluorobenzene, belongs to bromides-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 138526-69-9, Product Details of 138526-69-9

At room temperature, dry diethyl malonate (1140.2 g, 7.12 mol) is initially charged in a 1.6 l apparatus with anchor stirrer, and sodium ethoxide (244.5 g, 3.59 mol) is added as a solid. Owing to the energy of reaction released, the internal temperature increases to about 60 C. After the reaction has ended, the ethanol formed is distilled off under reduced pressure (400 mbar) and simultaneous increase of the temperature from 60 to 80 C. At 80 C., the pressure is gradually reduced to 10 mbar. At atmospheric pressure, the residue is then cooled to 75 C., and CuBr (53.4 g, 0.37 mol) and 3,4,5-trifluorobromobenzene (338.4 g, 1.60 mol) are then added successively over a period of 20 minutes, and the mixture is kept at 75 C. for another 18 hours. After the reaction has ended, the reaction mixture is cooled to 15 C. and, with stirring, added to a mixture, cooled to 10 C., of hydrochloric acid (36% strength, 260.9 g) and water (512.8 g). The reaction mixture obtained is filtered. Following separation of the phases of the filtrate, water (512.8 g) is added to the organic phase, and the pH is adjusted to 3.8 by addition of potassium carbonate (5.9 g, 50% strength solution in water). The phases are separated again, and the organic phase is then freed from volatile components under reduced pressure (0.5 mbar) up to an internal temperature of 127 C. According to quantitative 19F-NMR spectroscopy, 79.6% of the residue (478.4 g) consisted of diethyl 3,4,5-trifluorophenylmalonate. This corresponds to a diethyl 3,4,5-trifluorophenyl-malonate yield of 82.0%.

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-3,4,5-trifluorobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; BASF SE; US2010/56820; (2010); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Related Products of 138526-69-9, 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. 138526-69-9, name is 1-Bromo-3,4,5-trifluorobenzene belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

After adding iodine (10.0 mg, 40.0 mumol) to a tetrahydrofuran solution (190 ml) of magnesium (5.76 g, 237 mmol), 3,4,5-trifluorobromobenzene (50.0 g, 237 mmol) was added at room temperature Was slowly added dropwise.After stirring at the same temperature for 30 minutes, a tetrahydrofuran solution (160 ml) of iodine (66.1 g, 261 mmol) was added at 0 C., and the mixture was stirred at room temperature for 2 hours.The reaction mixture was poured into ice water, neutralized with concentrated hydrochloric acid, and extracted with hexane. The extract was washed with saturated aqueous sodium thiosulfate solution, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The concentrate was purified by silica gel column chromatography (eluent: ethyl acetate / n-hexane = 1/10) to give the title compound as a yellow oil (yield 45.0 g, yield 70%).

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-3,4,5-trifluorobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Hokko Chemical Industry Co., Ltd.; Suzuki, Jun; Wakabayashi, Jin; Murakami, Hideyuki; Onoue, Shinji; (19 pag.)JP2016/84348; (2016); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Electric Literature of 138526-69-9, 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. 138526-69-9, name is 1-Bromo-3,4,5-trifluorobenzene, This compound has unique chemical properties. The synthetic route is as follows.

Addition of iodine to a mixture of magnesium (264 mg, 11.0 mmol) and THF (5 mL)(5.0 mg) and 5-bromo-1,2,3-trifluorobenzene in THF (0.5 mL)(211 mg, 1 mmol) solution. The mixture is heated to 60 C,And 5-bromo-1,2,3-trifluorobenzene added dropwise in THF (4.5 mL)(1.9 g, 9 mmol) solution. The reaction is heated for two hours,The solution was cooled to room temperature and used directly in the next step.

The chemical industry reduces the impact on the environment during synthesis 1-Bromo-3,4,5-trifluorobenzene. I believe this compound will play a more active role in future production and life.

Reference:
Patent; PFIZER INC.; KUMPF, ROBERT ARNOLD; MCALPINE, INDRAWAN JAMES; MCTIGUE, MICHELE ANN; PATMAN, RYAN; RUI, EUGENE YUANJIN; TATLOCK, JOHN HOWARD; TRAN-DUBE, MICHELLE BICH; WYTHES, MARTIN JAMES; (445 pag.)TW2018/2074; (2018); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Synthetic Route of 138526-69-9, A common heterocyclic compound, 138526-69-9, name is 1-Bromo-3,4,5-trifluorobenzene, molecular formula is C6H2BrF3, 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.

General procedure: A mixture of the styrene (3 mmol), the halogenated benzene (3 mmol), triethanolamine (3 mmol) and Pd (II) acetate (0.03 g) was stirred under argon at 100 C for 24 h. The reaction was cooled to 25 C, quenched by the addition of dil. aq. hydrochloric acid (2 N, 10 ml), and extracted with ether (3 × 100 ml). The organic phases were dried (Na2SO4), the solvents evaporated, and the crude product was subjected to chromatography (silica gel, hexane/ethyl acetate mixtures).

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:
Article; Csuk, Rene; Albert, Sabrina; Siewert, Bianka; Schwarz, Stefan; European Journal of Medicinal Chemistry; vol. 54; (2012); p. 669 – 678;,
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. 138526-69-9, name is 1-Bromo-3,4,5-trifluorobenzene, This compound has unique chemical properties. The synthetic route is as follows., Application In Synthesis of 1-Bromo-3,4,5-trifluorobenzene

2L three-necked flask, nitrogen protection, cast diisopropylamine, tetrahydrofuran 750g,Cooling -40 dropping n-butyl lithium, dropping temperature insulation reaction 30min, cooling to -78 , dropping raw materials3,4,5, -trifluorobromobenzene, dropping off,-78 insulation 2h.The temperature was raised to -60 C began dropping dimethyl sulfate,Maintain the temperature is not higher than -30 , the dropping was completed naturally rose to room temperature, incubated for 30min.Stop the reaction, the pump off the pressure of tetrahydrofuran,Add 400g of water,Dichloroethane extraction, the organic phase was washed again, concentrated under reduced pressure distillation, to obtain the final product 2-methyl-3,4,5-trifluorobromobenzene purity of 99.5% or more, a yield of 61%.

According to the analysis of related databases, 138526-69-9, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Bengbu Zhong Shi Chemical Co., Ltd.; Yang Qing; Zhang Hao; Zhao Shimin; Xu Jianxiao; (4 pag.)CN105967974; (2016); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Synthetic Route of 138526-69-9, 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. 138526-69-9, name is 1-Bromo-3,4,5-trifluorobenzene belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: The amount ratio of the charged material is 3,4,5-trifluorobromobenzene: trimethyl borate = 1:1; Precipitating 28.476 g (0.14 mol) of 3,4,5-trifluorobromobenzene in 70 mL of tetrahydrofuran,Formulation to form a 3,4,5-trifluorobromobenzene solution.In a 1000 mL dry three-necked flask equipped with a thermometer and a constant pressure dropping funnel, 3.8 g of magnesium dust was added.(0.16mol),Tetrahydrofuran (30 mL), 1 mL of 1,2-dibromoethane and 5 mL of the above-prepared 3,4,5-trifluorobromobenzene solution were added dropwise under N2 protection.When the reaction is initiated at 5 to 10 C, a large amount of bubble temperature rises rapidly, and the solution slowly turns grayish black.And controlling the temperature to drop the remaining 3,4,5-trifluorobromobenzene solution (80 mL) of the above configuration at 10 C,The solution slowly turned black-gray, and after the addition was completed, it was kept at 25 C for 2 h.The reaction solution is then cooled to below -30 C (ie, the temperature at which the format reagent reacts with trimethyl borate),Adding a solution of trimethyl borate (dissolving trimethyl borate (14.56 g, 0.14 mol) in 50 mL of tetrahydrofuran to prepare a solution),And keep the temperature stable at -30 ~ -27 C, after the addition of trimethyl borate solution, continue the insulation reaction for 2h.Then, 135 mL of dilute hydrochloric acid having a concentration of 12% was added dropwise to the reaction solution, and the mixture was hydrolyzed at room temperature for 4 hours.After the completion of the hydrolysis reaction, ethyl acetate was added to the reaction mixture to extract a layer (50 mL × 3), and the extract phase was combined.The extract phase was dried over anhydrous sodium sulfate, and the solvent was evaporated to concentrate.Suction filtration to give a small amount of white solid washed with dichloromethane, and dried to give 10.8 g of white powder,That is, 3,4,5-trifluorobenzeneboronic acid represented by the formula (II) was obtained in a yield of 44%.

The synthetic route of 1-Bromo-3,4,5-trifluorobenzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Zhejiang University of Technology; Li Zhenhua; Zhang Xuchao; Tan Zhiyong; (11 pag.)CN109761820; (2019); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Electric Literature of 138526-69-9,Some common heterocyclic compound, 138526-69-9, name is 1-Bromo-3,4,5-trifluorobenzene, molecular formula is C6H2BrF3, 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: An argon filled 50 mL two-necked flaskequipped with a stir bar and a gas condenser was charged withmagnesium turnings (129 mg, 5.300 mmol). After three successivevacuum/argon cycles, THF (15 mL) and one grain of iodine wereadded, and the brownish suspensionwas stirred for 15 min at roomtemperature. Subsequently fluorinated bromobenzene(5.200 mmol) was added. An exothermic reaction was followed bychanges of the color of the reaction mixture from original brown,through colorless to final grayish. This suspensionwas stirred 2 h atroom temperature and then 3-phenylisobenzofuran-1(3H)-one(19) (1.000 g, 4.757 mmol) was added and stirring continued for16 h. Then Ac2O (4 mL) was added dropwise and the reactionmixture was refluxed at the temperature of the oil bath 70 C foradditional 30 min. A dense yellowish precipitate was formed. Theyellow suspension was cooled to room temperature, diluted withether (100 mL), and washed with a saturated aqueous solution ofNaHCO3 (3 15 mL). The deep yellow organic phase was dried overMgSO4. Solvents were removed under reduced pressure and columnchromatography on silica gel (hexane/ethyl-acetate – 4:1)afforded products as yellow crystalline solids.

The synthetic route of 138526-69-9 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Kaleta, Ji?i; ?imkova, Ludmila; Li?ka, Alan; Bim, Daniel; Madridejos, Jenica M.L.; Pohl; Ruli?ek, Lubomir; Michl; Ludvik, Ji?i; Electrochimica Acta; vol. 321; (2019);,
Bromide – Wikipedia,
bromide – Wiktionary

Electric Literature of 138526-69-9, The chemical industry reduces the impact on the environment during synthesis 138526-69-9, name is 1-Bromo-3,4,5-trifluorobenzene, I believe this compound will play a more active role in future production and life.

General procedure: In a typical experiment a dry and argonflushed50-mL Schlenk tube, equipped with a magnetic stirring bar, was charged with therespective fluorinated bromobenzene derivative (0.5 mmol, 88 mg for monosubstituted, 97 mgfor disubstituted and 105 mg for trisubstituted derivatives) and 3 mol% of the respective catalystdissolved in 15 ml of THF ([FeCl2(dppe)]: 7.9 mg, [FeCl2(dppp)]: 8.1 mg, [NiCl2(dppm)]: 7.7mg, [NiCl2(dppe)]: 7.9 mg, [NiCl2(dppp)]: 8.1 mg, [PdCl2(dppm)]: 8.4 mg, [PdCl2(dppe)]: 8.6mg, [PdCl2(dppp)]: 8.8 mg). The solution was stirred for 5 min, then cyclohexyl magnesiumbromide or the respective LiCl or LiBr adduct (0.8 mmol, 4 ml of a 0.2M Grignard reagent) wasquickly added to the reaction mixture and vigorous stirring at room temperature was continuedfor 24 hours. After hydrolysis with diluted hydrochloric acid, the organic layer and ether extractsfrom the aqueous layer were combined, washed with water and saturated NaCl solution, driedover MgSO4 and filtrated through a pad of silica. Concentration under reduced pressure followedby column chromatography (hexane : diethyl ether, v/v 100 : 1) afforded the respective coupling products as light yellow oily compounds

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-3,4,5-trifluorobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Dahadha, Adnan; Imhof, Wolfgang; ARKIVOC; vol. 2013; 4; (2013); p. 200 – 216;,
Bromide – Wikipedia,
bromide – Wiktionary

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. 138526-69-9, name is 1-Bromo-3,4,5-trifluorobenzene belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Product Details of 138526-69-9

(a) To 50 ml of N-methylpyrrolidone were added 10 g of 3,4,5-trifluorobromobenzene and 8.5 g of copper cyanide, and the resulting mixture was stirred at 150C for 4 hours. Thereafter, aqueous ammonia was added to the reaction mixture which had been allowed to cool to near room temperature, followed by extraction with ethyl acetate. The organic layer was dried over magnesium sulfate, and concentrated under reduced pressure. The residue was subjected to silica gel column chromatography, and 5.0 g of 3,4,5-trifluorobenzonitrile was obtained.

The synthetic route of 138526-69-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Sumitomo Chemical Company, Limited; EP2151432; (2010); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Electric Literature of 138526-69-9, A common heterocyclic compound, 138526-69-9, name is 1-Bromo-3,4,5-trifluorobenzene, molecular formula is C6H2BrF3, 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.

General procedure: PN (0.004 mol) was dissolved in anhydrous tetrahydrofuran (10 mL). The solution was added dropwise to the appropriate Grignard reagent (0.006 mol, 1 mol/L in tetrahydrofuran, prepared from respective bromide and magnesium) via a syringe at -40 C. After stirring for 20 min, the reaction was moved to ice-bath and quenched with saturated aqueous solution of ammonium chloride. The aqueous phase was extracted with dichloromethane and the combined organic layer was washed with brine, dried over anhydrous sodium sulfate. The solvent was evaporated and the residue was dissolved in dichloromethane and treated with DDQ (0.004 mol). The reaction was refluxed for 3 h, filtered to move the precipitate. The crude product was further purified by column chromatography (petrol ether: ethyl acetate = 5:1) [21].

The synthetic route of 138526-69-9 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Zhang, Ya-Nan; Feng, Yi-An; Li, Zhong; Shao, Xu-Sheng; Chinese Chemical Letters; vol. 28; 6; (2017); p. 1228 – 1231;,
Bromide – Wikipedia,
bromide – Wiktionary