Category: bromides-buliding-blocks

Synthetic Route of 955959-84-9, 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 955959-84-9 as follows.

In a round bottom flask, 4.9 g of aniline, 30 g of starting material X1, t-BuONa 14.5 g, Pd2(dba)3 2.2 g, and (t-Bu)3P 2.3 m were dissolved in 200 ml of toluene, stirred at reflux. The reaction was confirmed by thin layer chromatography (TLC), and after adding water, the reaction was terminated. Use methyl cellulose (MC) to extract organic layers and reduce themAfter pressure filtration, column purification and recrystallization were carried out to obtain 16.2 g (yield 81percent) of IA-1.

According to the analysis of related databases, 955959-84-9, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Dongjin Shimeiken Co., Ltd.; Jin Jintai; Xian Haowan; Jin Dongjun; Lin Donghuan; Li Yingzhen; Lin Dazhe; Han Zhengyou; Pei Weizhen; Jin Yingsen; Li Dongxuan; (49 pag.)CN108689913; (2018); A;,
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Related Products of 553-94-6, 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. 553-94-6, name is 2,5-Dimethylbromobenzene belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

In a 250mL dry four-neck flask, evacuate and replace the system three times with nitrogen, and then add 60mL of anhydrous ether, 3.77g of magnesium filings (molecular weight 24.3, 155.20mmol, 1.2eq) and a small iodine (15mg) under nitrogen protection. ), Raise the temperature to 60 C, and slowly add about one-fifth of a solution of 2,5-dimethylbromobenzyl ether [25.75g of 2,5-dimethylbromobenzyl (molecular weight 199.09, 129.33mmol) , 1eq) dissolved in 30mL of ether], the temperature did not increase significantly, stirred at this temperature for about 30 minutes, at this time observed the temperature rose significantly, reached a reflux state, at the same time the yellow in the solution faded and turned off-white. The remaining 2,5-dimethylbromobenzyl ether solution was slowly added dropwise, and the drop was completed in about 40 minutes. After dripping and holding for 1 hour, it was observed that the magnesium dust in the reaction solution had basically disappeared. The temperature of the reaction solution was lowered to 0 C, and 46.04 g of ethylene oxide (molecular weight 44.05, 1034.6 mmol, 8.0 eq) was slowly added. After the addition, the temperature was maintained at about 0 C and stirring was continued for 3 hours. 70 mL of saturated ammonium chloride solution was added to extract the reaction. After the tetrahydrofuran was distilled off under negative pressure, the aqueous phase was extracted three times with 40 mL of dichloromethane. The dichloromethane phases were combined and the dichloromethane was evaporated to dryness under negative pressure to obtain 18.87 g (molecular weight 150.22, theoretically obtained). 19.43 g) a white solid. The purity was 97.5%, which was 2,5-dimethylphenylethanol, and the mass yield was 94.69%.

The synthetic route of 2,5-Dimethylbromobenzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Jiangsu Zhongqi Technology Co., Ltd.; Wu Yaojun; Bu Long; Zhang Pu; Hou Yuanchang; (7 pag.)CN110357774; (2019); A;,
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Electric Literature of 583-70-0, 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. 583-70-0, name is 2,4-Dimethylbromobenzene belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Examples 42-45 Bis-(2,4-dimethylphenyl)chlorophosphine (B42): A solution of 2.92 ml (2161 mmol) of 4-bromo-1,3-dimethylbenzene in 3 ml of Et2O were added at 0 C. to a suspension of 0.5 g (20.56 mmol) of magnesium turnings in 7 ml of THF and 7 ml of Et2O and also a crystal of iodine. The mixture was heated to room temperature, stirred further overnight and slowly added dropwise at 0 C. to a solution of 1.5 ml (10.31 mmol) of Et2NPCl2 in 8 ml of THF. The mixture was heated to room temperature and the solvent was subsequently removed under reduced pressure. After adding 60 ml of hexane, the mixture was filtered through Celite under argon and admixed with hydrogen chloride for 1 hour. After degassing, the resulting solids were filtered off under argon and dried. Yield: 1.4 g (58.3% of theory). 1H NMR (400 MHz, CDCl3) delta, 7.40 (d, Jmeta=4.5 Hz, 2H, arom.), 7.2 (m, 4H, arom.), 2.5 (d, JPH=2.0 Hz, 6H, CH3), 2.4 (s, 6H, CH3). 31P NMR (161.974 MHz, CDCl3) delta, 75.6.

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, 2,4-Dimethylbromobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Meseguer, Benjamin; Militzer, Hans-Christian; Castillon, Sergio; Claver, Carmen; Diaz, Yolanda; Aghmiz, Mohamed; Guiu, Ester; Aghmiz, Ali; Masdeu, Anna; US2005/80047; (2005); A1;,
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22385-77-9, name is 1-Bromo-3,5-di-tert-butylbenzene, belongs to bromides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. COA of Formula: C14H21Br

Bromo-3,5-di-tert-butylbenzene (1.3 g, 5 mmole) was dissolved in THF (20 mL), to this solution was slowly added n-BuLi (1.6 M, 3.3 mL) at -78° C., the reaction was stirred at this temperature for 30 min, trimethyl borate (0.75 g, 7.5 mmole) was added all at once, stir over night while the reaction was allowed to slowly warm up to room temperature. Hydrochloric acid (6N, 5 mL) was added and stirred for 3 hrs at room temperature. Water (200 mL) was added, and the precipitate was collected, washed with water (10 mL.x.3), dried under vacuum to give titled compound.

The synthetic route of 22385-77-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Adams, Alan D.; Santini, Conrad; US2009/30012; (2009); A1;,
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Related Products of 108-85-0, The chemical industry reduces the impact on the environment during synthesis 108-85-0, name is Bromocyclohexane, I believe this compound will play a more active role in future production and life.

General procedure: Benzo[b]thiophene-3-carbaldehyde (40 mg, 0.25 mmol, 1.0 equiv),Pd(TFA) 2 (4.2 mg, 5 mol%), (4-FC 6 H 4 ) 3 P (9.5 mg, 12 mol%), DPEphos (8mg, 6 mol%), and Cs 2 CO 3 (122 mg, 0.375 mmol) were placed in atransparent Schlenk tube equipped with a stirring bar. The tube wasevacuated and filled with argon for three times. Degassed DMF (2.5mL) and tert-butyl bromide (51 mg, 0.375 mmol, 1.5 equiv) were add-ed via a gastight syringe. The reaction mixture was stirred under theirradiation of 36 W blue LEDs (distance app. 2.0-3.0 cm from thebulb) at r.t. for 24 h. The mixture was quenched with brine and ex-tracted with EtOAc (3 × 10 mL). The organic layers were combinedand concentrated under reduced pressure. The product was purifiedby flash column chromatography on silica gel using PE or a mixture of PEand EtOAc (10:1 v/v) as eluent; yield: 50.1 mg (92%); pale yellow liquid.

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, Bromocyclohexane, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Wang, Guang-Zu; Shang, Rui; Fu, Yao; Synthesis; vol. 50; 15; (2018); p. 2908 – 2914;,
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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. 153505-37-4, name is 4-Bromo-5-fluorobenzene-1,2-diamine belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Formula: C6H6BrFN2

4-bromo-5-fluorobenzene-1,2-diamine (5.00 g, 24.4 mmol) was solubilised in 1 ,4-dioxane (200 ml). 4,4,4′,4′,5,5,5′,5′-octamethyl-2,2′-bi-1,3,2-dioxaborolane (7.43 g, 29.3 mmol), potassium acetate (12.0 g, 122 mmol) and dichlorobis(tricyclohexylphosphine)palladium(ll) (900 mg, 1 .22 mmol) were added and the mixture was stirred overnight at 1 10C. The mixture was filtered and the filtrate was concentrated under reduced pressure. The crude mixture was purified by flash chromatography on silica gel to give 3.23 g (90 % purity, 47 % yield) of the title compound. LC-MS (Method 2): Rt = 0.75 min; MS (ESIpos): m/z = 253 [M+H]+ 1H-NMR (400 MHz, DMSO-d6) _ [ppm]: 1.066 (0.59), 1 .156 (2.87), 1 .230 (16.00), 5.191 (1.07), 6.172 (1.00), 6.200 (1.04), 6.739 (0.89), 6.755 (0.89).

The synthetic route of 153505-37-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BAYER PHARMA AKTIENGESELLSCHAFT; LEFRANC, Julien; MENGEL, Anne; SCHULZE, Volker; CHRIST, Clara; PRINZ, Florian; WENGNER, Antje, Margret; STOeCKIGT, Detlef; BOeMER, Ulf; BADER, Benjamin; (288 pag.)WO2017/207534; (2017); A1;,
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Application of 452-74-4, A common heterocyclic compound, 452-74-4, name is 1-Bromo-2-fluoro-4-methylbenzene, molecular formula is C7H6BrF, 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.

3-Fluoro-4-bromotoluene (5.0 g, 27 mmol) in carbon tetrachioride (50 mE) was treated with N-bromosuccinimide (7.0 g, 40 mmol, 1.5 eq) and heated to 80 C. Henzoyl peroxide (65 mg, 0.27 mmol, 0.01 eq.) was added and heating was continued for 1 h. The reaction was then cooled to ambient temperature and filtered, and the filtercake was washed sparingly with chloroform. The filtrate was washed with water and brine, dried over Na2SO4, and concentrated to give crude 3-fluoro-4-bromobenzyl bromide as a clear oil which was used without thrther 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; INFINITY PHARMACEUTICALS, INC.; BEHNKE, Mark L.; CASTRO, Alfredo C.; EVANS, Catherine A.; GRENIER, Louis; GROGAN, Michael J.; LIU, Tao; SNYDER, Daniel A.; TIBBITTS, Thomas T.; US2015/368278; (2015); A1;,
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Some common heterocyclic compound, 583-75-5, name is 4-Bromo-2-methylaniline, molecular formula is C7H8BrN, 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. Computed Properties of C7H8BrN

EXAMPLE 192 1,2-Dihydro-6-(3-nitrophenyl)-2,2,4,8-tetramethylquinoline (Compound 292, structure 86 of Scheme XXII, where R1 =R3-5 =H, R2 =nitro) 4-Bromo-2-methylaniline (5.58 g, 30 mmol) was treated with iodine (0.2 g, 0.9 mmol) and acetone (150 mL) in a sealed tube at. 80 C. for 24 h to provide 6-bromo-1,2-dihydro-8-methylquinoline (Compound 85 of Scheme XXII) in 9% yield as a yellow oil (0.70g). Most of the aniline (>80%) was recovered.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 583-75-5, its application will become more common.

Reference:
Patent; Ligand Pharmaceuticals Incorporated; US5696130; (1997); A;,
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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. 138526-69-9, name is 1-Bromo-3,4,5-trifluorobenzene, A new synthetic method of this compound is introduced below., SDS of cas: 138526-69-9

The format reagent is kept at a reaction temperature of 5 C.3,4,5-trifluorobromobenzene 28.476 g (0.14 mol) was previously dissolved in 70 mL of THF to prepare a 3,4,5-trifluorobromobenzene solution.Trimethyl borate (64.4 g, 0.28 mol) was previously dissolved in THF (50 mL) to form a trimethyl borate solution.In a 1000 mL dry three-necked flask equipped with a thermometer and a constant pressure dropping funnel,Add 3.8 g (0.16 mol) of magnesium, THF (30 mL),Under the protection of N2, 1 mL of 1,2-dibromoethane and 5 mL of the above-mentioned 3,4,5-trifluorobromobenzene solution were added dropwise, and the reaction was initiated at 5 to 10 C, and a large amount of bubble temperature rose rapidly. Slowly turned grayish black,And controlling the temperature to drop the remaining 3,4,5-trifluorobromobenzene solution of the above configuration at 10 C, the solution slowly turns black gray, after the addition is completed,The reaction was incubated at 5 C for 2 h (ie, the format reagent was kept at a reaction temperature of 5 C).Then the reaction solution is cooled to about -30~-27 C.The above-prepared trimethyl borate solution was slowly added dropwise dropwise.After the completion of the dropwise addition, the reaction was continued at -30 C for 2 h.After the reaction was completed, dilute hydrochloric acid (135 mL of 12% dilute hydrochloric acid) was added dropwise at room temperature, and the mixture was stirred at room temperature for 4 h.Ester extraction (50 mL × 3), the organic phase is combined, dried over anhydrous sodium sulfate, and the organic phase is distilled off under reduced pressure, and the residue is distilled.Add 20 mL of dichloromethane, stir for 5 min, filter with a white solid, wash with a small amount of dichloromethane, and dry to give a white powder3,4,5-trifluorobenzeneboronic acid 14.78 g, yield 60%.

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; Zhejiang University of Technology; Li Zhenhua; Zhang Xuchao; Tan Zhiyong; (11 pag.)CN109942433; (2019); A;,
Bromide – Wikipedia,
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Electric Literature of 111721-75-6,Some common heterocyclic compound, 111721-75-6, name is 2-Bromo-3-fluoroaniline, molecular formula is C6H5BrFN, 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 stirred solution of 2-bromo-3-fluoro aniline (25.0 g, 131.57 mmol) in dichloromethane (500 mL) at 0 C under nitrogen was added acetic anhydride (18.65 mL, 197.36 mmol). The resulting mixture was warmed to room temperature and stirred for 16 hours. After that, the reaction mixture was diluted water and extracted with dichloromethane (2 x 500 mL). The combined organic phase was washed with brine, dried over anhydrous Na2S04 and concentrated in vacuo to get compound XlVa (crude), which was taken as such for the next step without further purification. Yield: 25 g, 81.91%. LC- MS Calc. for C8H7BrFNO, 232.05; Obs.; 232.0 [M+]; -NMR (300 MHz, DMSO-d6): delta 9.57 (s, 1H), 7.49-7.34 (m, 2H), 7.20-7.14 (m, 1H), 2.09 (s, 3H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2-Bromo-3-fluoroaniline, its application will become more common.

Reference:
Patent; BUGWORKS RESEARCH INDIA PVT LTD; PEER MOHAMED, Shahul Hameed; BHARATHAM, Nagakumar; KATAGIHALLIMATH, Nainesh; SHARMA, Sreevalli; NANDISHAIAH, Radha; RAMACHANDRAN, Vasanthi; VENKATARAMAN, Balasubramanian; (221 pag.)WO2018/225097; (2018); A1;,
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