Bromides-buliding-blocks

583-75-5, These common heterocyclic compound, 583-75-5, name is 4-Bromo-2-methylaniline, 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.

3,6-Dibromotoluene In a 2000 ml beaker containing 400 ml of 23percent aqueous HBr, 46.5 g (0.25 mol) of melted 2-methyl-4-bromoaniline was slowly added. This mixture was stirred for 20 minutes using a mechanical stirrer, then cooled to -5¡ã C. Then a solution of 22.4 g (0.33 mol) of NaNO2 in 130 ml of water was added dropwise over 1 hour at this temperature. The diazonium reagent obtained was added in several portions to a solution of 35.9 g (0.25 mmol) of CuBr in 100 ml of 47percent HBr at 0¡ã C. The resulting mixture was warmed to 70¡ã C., stirred for 30 minutes at this temperature, and, then, cooled to room temperature. The product was extracted with 3*200 ml of methyl-tert-butyl ether. The combined extract was dried over K2CO3 and evaporated to dryness. Firstly, the crude product was purified using short column with Silica Gel 60 (40-63 mum, d 60 mm, 140 mm; eluant: hexanes). Fractional distillation gave colorless oil, b.p. 100-102¡ã C./10 mm Hg. Yield, 36.1 g (58percent). Anal. calc. for C7H6Br2: C, 33.64; H, 2.42. Found: C, 33.79; H, 2.50. 1H NMR (300 MHz, CDCl3): delta 7.39 (m, 1H, 5-H), 7.37 (m, 1H, 3-H), 7.18 (m, 1H, 6-H), 2.38 (s, 3H, Me). 13C NMR (75 MHz, CDCl3): delta 139.9, 133.6, 133.5, 130.3, 123.5, 120.9, 22.7.

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 583-75-5.

Reference:
Patent; Voskoboynikov, Alexander Z.; Izmer, Vyatcheslav V.; Asachenko, Andrey F.; Nikulin, Mikhail V.; Ryabov, Alexey N.; Lebedev, Artyom Y.; Coker, Catalina L.; Canich, Jo Ann M.; US2007/135597; (2007); A1;,
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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 10269-01-9 as follows. 10269-01-9

A solution of (3-bromophenyl)methanamine (1 g, 5.37 mmol) in dichloromethane (10 mL) at 10 C. was treated with triethylamine (1 .498 mL, 10.75 mmol) then fe/ -butyl dicarbonate (1 .498 mL, 6.45 mmol) and stirred at 10 C for 4 h. Water (10 mL) was added then the mixture extracted with DCM (2 x 10 mL), washed with brine, dried and evaporated and the residue purified by chromatography (silica gel, 10:1 hexanes/ethyl acetate) to afford the desired product (1 .5 g; 93%) as a colorless solid. NMR (500 MHz, CDCI3) delta ppm 7.43 (s, 1 H), 7.39 (d, J = 6.8 Hz, 1 H), 7.20 (d, J = 6.8 Hz, 2H), 4.89 (s, 1 H), 4.29 (d, J = 5.7 Hz, 2H), 1 .46 (s, 9H).

According to the analysis of related databases, 10269-01-9, the application of this compound in the production field has become more and more popular.

Reference:
Patent; GLAXOSMITHKLINE INTELLECTUAL PROPERTY DEVELOPMENT LIMITED; DUFFY, Kevin J.; PARRISH, Cynthia Ann; ATOR, Laura E.; BASKARAN, Subramanian; DARCY, Michael Gerard; OPLINGER, Jeffrey Alan; RALPH, Jeffrey M.; RIDGERS, Lance Howard; TIAN, Xinrong; ZHANG, Cunyu; (225 pag.)WO2019/53617; (2019); A1;,
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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. 18869-30-2, name is (E)-1,2-Bis(4-bromophenyl)ethene belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. 18869-30-2

EXAMPLE 3 Ethyl 4-bromostilbene-4′-acrylate. 25.8 g (0.1 mol) of 4,4′-dibromostilbene, 10 g (0.1 mol) of ethyl acrylate, 18.5 g (0.1 mol) of tri-n-butylamine, 0.224 g (0.001 mol) of palladium acetate and 0.6 g (0.002 mol) of tri-o-tolylphosphine are added under argon to 50 ml of p-xylene. The reaction mixture is stirred at 90 C. for 4 hours. Working up gives 2 g (6% of theory) of ethyl 4-bromostilbene-4′-acrylate. Melting point 166.9 C.

The synthetic route of 18869-30-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Ciba-Geigy Corporation; US4918215; (1990); A;,
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626-39-1, Adding a certain compound to certain chemical reactions, such as: 626-39-1, name is 1,3,5-Tribromobenzene, 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 626-39-1.

Carbazole (6.6 g, 39.7mmol), 1,3,5-tribromobenzene (5 g, 15.9mmol), cuprous iodide (0.3 g,1.6 mmol), potassium phosphate (13.7 g, 64.5 mmol) and trans-1,2-cyclohexanediamine(1.6 g, 15.9 mmol) were dissolved in 200 mL of 1,4-dioxane. After the mixed solution wasstirred in a nitrogen atmosphere for 19 h at 110C, the reaction mixture was cooled to roomtemperature. The mixture extracted with dichloromethane (80 mL ¡Á 3 times) and driedover anhydrous MgSO4. The crude product was subjected to flash column chromatography(dichloromethane: n-hexane = 1: 4) to give compound (1) (6.3 g, 79%). 1H NMR (CDCl3,300MHz); delta = 7.68 (d, -CH-), 7.5 (d, -CH-), 7.45 (d, -CH-), 7.35 (m-CH-), 7.29(t, -CH3),7.18(m, -CH-).

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

Reference:
Article; Yun, Seong-Jae; Seo, Minhye; Lee, Sungkoo; Molecular Crystals and Liquid Crystals; vol. 662; 1; (2018); p. 82 – 90;,
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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. 22034-13-5, name is 4-Bromobenzo[c][1,2,5]thiadiazole belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. 22034-13-5

4-Bromobenzo [c] [1,2,5] thiadiazole (100 g, 0.46 mol),4,4,4?,4?,5,5,5?,5?-octamethyl-2,2?-bi-1,3,2-dioxaborolane(141 g, 0.55 mol), Pd (dppf) Cl2 (32 g, 0.04 mol) and KOAc (90 g, 0.92 mol) were placed in a flask, To this was added 1,4-dioxane (2 L) and dissolved, followed by heating and stirring for 8 hours. After completion of the reaction, Distilled water was added and the organic layer was extracted with ethyl acetate.The obtained organic layer was dried over Na2SO4, distilled under reduced pressure,Purification by column chromatography afforded compound 4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)benzo[c][1,2,5]thiadiazole(72 g, yield 60percent) was obtained as white crystals.

The synthetic route of 22034-13-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Doosan Co., Ltd; Choi Tae-jin; (52 pag.)KR2018/71882; (2018); A;,
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402-43-7, 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 402-43-7 as follows.

General procedure: Na2CO3 (212 mg, 2 mmol), 4-chloronitrobenzene (1 mmol) and styrene (1.5 mmol) were added successively into a dried Schlenk tube under nitrogen. Then the DMA (0.1 mL) solution of DADPP (0.002 mmol) and [Pd(C3H5)Cl]2 (0.0005 mmol), which was reacted at 100 C for 10 min prior to use, was added into the mixture. The reaction was performed at 130 C. At the end of reaction, the mixture solution was extracted with ethyl acetate (3 ¡Á 5 mL). Combined organic phase was washed with brine (3 ¡Á 5 mL) and dried over MgSO4. The dried solution was filtered and purified with silica gel chromatography (petroleum ether 60-90 C) to give a corresponding product.

According to the analysis of related databases, 402-43-7, the application of this compound in the production field has become more and more popular.

Reference:
Article; Jiang, Zhi-Jie; Wang, Wei; Zhou, Rong; Zhang, Lei; Fu, Hai-Yan; Zheng, Xue-Li; Chen, Hua; Li, Rui-Xiang; Catalysis Communications; vol. 57; (2014); p. 14 – 18;,
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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 615-59-8 as follows. 615-59-8

3,6-Dibromobenzylbromide In a 250 ml three-necked round-bottom flask equipped with a reflux condenser, thermometer, dropping funnel with pressure-equalizing, and magnetic stirring bar, and containing 74.9 g (0.30 mol) of 3,6-dibromotoluene, 15.5 ml (47.9 g, 0.30 mmol) of bromine was added dropwise under exposure to 500 W lamp for 3 hours at 190¡ã C. The resulting mixture was cooled to room temperature. Fractional distillation gave colorless liquid, b.p. 132-135¡ã C./3 mm Hg. Yield 84.3 g (85percent). Anal. calc. for C7H5Br3: C, 25.57; H, 1.53. Found: ¡ã C, 25.81; H, 1.62. 1H NMR (CDCl3): delta 7.59 (m, 1H, 5-H), 7.43 (m, 1H, 3-H), 7.28 (m, 1H, 3-H), 4.52 (s, 2H, CH2). 13C NMR (CDCl3): delta 138.9, 134.6, 134.0, 133.1, 123.0, 121.5, 32.2.

According to the analysis of related databases, 615-59-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Voskoboynikov, Alexander Z.; Ryabov, Alexey N.; Nikulin, Mikhail V.; Lygin, Alexander V.; Coker, Catalina L.; Canich, Jo Ann M.; US2007/135595; (2007); A1;,
Bromide – Wikipedia,
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Adding a certain compound to certain chemical reactions, such as: 17247-58-4, name is (Bromomethyl)cyclobutane, 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 17247-58-4, 17247-58-4

4e. Preparation of cyclobutylcarbinylsulfonamide A solution of 12.3 g (83 mmol) of cyclobutylcarbinyl bromide (Aldrich) and 13.7 g (91 mmol) of sodium iodide in 150 mL of acetone was refluxed overnight and then cooled to room temperature. The inorganic solids were filtered off and the acetone and cyclopropylcarbinyl iodide (8.41 g, 46%) distilled off at ambient and 150 torr at 80 C., respectively. A solution of 4.0 g (21.98 mmol) of cyclobutyl carbinyl iodide in 30 mL of anhydrous diethyl ether (diethyl ether) cooled to -78 C. was cannulated into a solution of 17 mL (21.98 mmol) of 1.3M sec-butyllithium in cyclohexanes and the solution was stirred for 5 minutes. To this mixture was cannulated a solution of 3.0 g (21.98 mmol) of freshly distilled sulfuryl chloride in 110 mL of hexanes cooled to -78 C., the mixture warmed to room temperature over 1 hour and was then carefully concentrated in vacuo. This mixture was redissolved in diethyl ether, washed once with some ice-cold water, dried (MgSO4), filtered, and concentrated carefully. This mixture was redissolved in 30 mL of THF, added dropwise to 500 mL of saturated NH3 in THF and was allowed to stir overnight. The mixture was concentrated in vacuo to a crude yellow solid and was recrystallized from the minimum amount of dichloromethane in hexanes with 1-2 drops of methanol to afford 1.39 g (42%) of cyclobutyl carbinylsulfonamide as a white solid. 1H NMR (CDCl3) delta 1.81-2.03 (m, 4H), 2.14-2.28 (m, 2H), 2.81-2.92 (m, 1H), 3.22 (d, J=7 Hz, 2H), 4.74 (brs, 2H); 13C NMR (CDCl3) delta 19.10, 28.21, 30.64, 60.93; MS m/e 148 (M-1)-. time: 1.73, method B), 818 (M++H)

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, (Bromomethyl)cyclobutane, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Sin, Ny; Good, Andrew Charles; Venables, Brian Lee; Scola, Paul Michael; Meanwell, Nicholas A.; US2006/183694; (2006); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Adding a certain compound to certain chemical reactions, such as: 656-64-4, name is 3-Bromo-4-fluoroaniline, 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 656-64-4, 656-64-4

N-Hydroxy-4-((2-methoxyethyl)amino)-1,2,5-oxadiazole-3-carbimidoyl chloride (1.5 kg, 6.8mol) was mixed with water (10 L). The mixture was heated to 60C. 3-Bromo-4-fluoroaniline (1.44 kg, 7.46 mol) was added and stirred for 10 mm. A warm sodium bicarbonate (0.86 kg, 10 mol)solution (10 L water) was added over 15 mm. The reaction mixture was stirred at 60C for 20 mm. The reaction mixture was cooled to room temperature and extracted with EtOAc (10 L*2). The combined organic solution was dried over sodium sulfate and concentrated to give the desired product (2.3 kg, 90%) as a brown solid. LCMS (M + H) : m / z = 374.0, 376.0. 1H NMR (400MHz, DMSO-d6): 6 11.55 (s, 1H), 8.85 (s, 1H), 7.16 (t, J = 8. 8Hz, 1H), 7.08 (dd, J = 6.1, 2.7Hz, 1H), 6.75 (m,1H), 6.14 (t, J = 5.8Hz, 1H), 3.48 (t, J = 5.2Hz, 2H), 3.35 (dd, J = 10.8, 5.6Hz, 2H), 3.22 (s, 3H).

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, 3-Bromo-4-fluoroaniline, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; GLAXOSMITHKLINE INTELLECTUAL PROPERTY DEVELOPMENT LIMITED; KAZMIERSKI, Wieslaw Mieczyslaw; DE LA ROSA, Martha; SAMANO, Vincent; (70 pag.)WO2017/2078; (2017); A1;,
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88223-35-2, 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. 88223-35-2, name is 2-Bromo-9,9-dibutyl-9H-fluorene belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

In a 250 mL round bottom flask was placed 7 (14.2 g, 40 mmol). The flask was evacuated under vacuum and flushed with nitrogen three times. THF (150 mL) was then added. The mixture was cooled to -78 C and n-BuLi (19.2 mL, 48 mmol) was slowly added. After the mixture was stirred for 5 h at -78 C, trimethyl borate (5.6 mL, 48 mmol) was injected. After 2 h, the mixture was slowly warmed to room temperature. HCl (3 M, 150 mL) solution was added and the mixture was stirred for another 3 h. The mixture was extracted with DCM three times. The combined organic layers were washed with water, dried over anhydrous sodium sulfate. The product was then dried under high vacuum. The crude product was condensed and purified on a silica-gel column using a mixture of DCM and acetone (5:1 by volume) as eluent. A white solid 4d (5.83 g, 45.3% yield) was obtained; m.p. 145-148 C. 1H NMR (300 MHz, d6-DMSO): delta (ppm): 7.98 (s, 2H), 7.83 (s, 1H), 7.74-7.82 (m, 3H), 7.43-7.45 (m, 1H), 7.31-7.34 (m, 2H), 1.95-1.99 (m, 4H), 0.98-1.06 (m, 4H), 0.61 (t, 6H, J = 7.5 Hz), 0.46-0.50 (m, 4H).

The synthetic route of 2-Bromo-9,9-dibutyl-9H-fluorene has been constantly updated, and we look forward to future research findings.

Reference:
Article; Zhu, Tianhao; He, Guangke; Chang, Jin; Zhao, Dongdong; Zhu, Xiaolin; Zhu, Hongjun; Dyes and Pigments; vol. 95; 3; (2012); p. 679 – 688;,
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