Category: bromides-buliding-blocks

Synthetic Route of 2695-47-8, 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. 2695-47-8, name is 6-Bromo-1-hexene belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To a two-neck oven-dried 250-mL round-bottom flask, 3,6-di(thiophen-2-yl)-2,5-dihydropyrrolo[3,4-c]pyrrole-1,4-dione(3.7 g, 12.2 mmol) and anhydrous K2CO3 (4.2 g, 30.5 mmol) were added. The reaction system was then evacuated and refilled with N2 before anhydrous DMF (50 mL) was injected by asyringe. After stirring and heating at 120C for 1 h, the temperatureof reaction mixture was decreased to 100C, after which6-bromohex-1-ene (5.0 g, 30.5 mmol) was added dropwise, and the reaction mixture was maintained at 100C with stirring for 2 days. After the reaction mixture was cooled to room temperature, it was poured into cold water and stirred for 30 min. The organic phase was extracted with dichloromethane, dried over anhydrous MgSO4, and then the crude product was subjected to column chromatography with hexane and chloroform as eluent. Additionally, a simple recrystallization from CHCl3/ethanol offered pure purple crystals (3.7 g, 65 %). deltaH (CDCl3, 400 MHz)8.90 (2H, d, J 3.6), 7.70 (2H, d, J 4.8), 7.31 (2H, t, J 4.8), 5.78-5.89 (2H, m), 4.49-5.04 (4H, m), 4.09 (4H, t, J 7.6), 2.09-2.15(4H, m), 1.72-1.79 (4H, m), 1.48-1.56 (6H, m).

The synthetic route of 6-Bromo-1-hexene has been constantly updated, and we look forward to future research findings.

Reference:
Article; Shi, Zugui; Neo, Wei Teng; Zhou, Hui; Xu, Jianwei; Australian Journal of Chemistry; vol. 69; 4; (2016); p. 403 – 410;,
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Application of 960203-41-2, A common heterocyclic compound, 960203-41-2, name is (2-Bromophenyl)(2,4-dimethylphenyl)sulfane, molecular formula is C14H13BrS, 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.

2.1 g of the compound C synthesized in Example 1 was charged into a 100 mL three-necked flask, and 0.9 g of piperazine, 0.3 g of cuprous iodide, 0.5 g of 2-acetylcyclohexanone and 3.0 g of potassium carbonate of 100 to 200 mesh were weighed into a flask, The amount of 50mL DMF into the flask,The reaction mixture was heated to reflux. TLC was used to detect the reaction. The reaction was complete with 100 mL of ethyl acetate and 150 mL of water. The filtrate was separated by suction filtration and the organic phase was washed twice with 100 mL of water. The organic phase was washed with anhydrous sulfuric acid After drying for 2 h, the oil was concentrated at 45 ° C to obtain an oil. After 30 mL of n-hexane was added to the oil, the mixture was stirred and crystallized for 3 h. After filtration, the filter cake was washed twice with a little solvent and the cake was vacuum dried at 40 ° C for 12 h. Brown solid product 2.2 g, yield 81.5percent.

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; Beijing Wanquan German public medicine Biotechnology Co., Ltd; Xu, Yong; Zhao, Guolei; (6 pag.)CN105367516; (2016); 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. 4263-52-9, name is Sodium 2-bromoethanesulphonate, A new synthetic method of this compound is introduced below., HPLC of Formula: C2H4BrNaO3S

44.6 g of isophorone diisocyanate (IPDI) was added in a mechanically agitated round-bottom flask. 0.2 mL of catalyst dibutyltin dilaurate was added in the IPDI, and 17.8 g of dimethyl ethanolamine (HO CH2CH2N(CH3)2) was added dropwise in the IPDI while stirring at 30 C. using a dropping funnel to form a reaction mixture. The reaction mixture reacted for 1 hr, and then was stirred to react for 12 hrs at 30 C. 42.2 g of 2-bromoethyl sodium sulfonate which was dissolved in 400 mL of anhydrous tetrahydrofuran was added dropwise in the reaction mixture and reacted for 1 hr to yield a white precipitate. The white precipitate was centrifugalized several times to yield the isocyanate-terminated betaine compound.

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; Shenzhen University; CHEN, Shiguo; YUAN, Lingjun; ZHU, Xingli; CHEN, Shaojun; GE, Zaochuan; (11 pag.)US2017/339960; (2017); A1;,
Bromide – Wikipedia,
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Application of 327-51-5, These common heterocyclic compound, 327-51-5, name is 1,4-Dibromo-2,5-difluorobenzene, 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.

Example i-7: methyl 5-fluoro-2-methoxy-4-(4,4,5,5-tetramethyl-l,3,2-dioxa borolan-2-yl)benzoate (i-7)Scheme i-7.i-7 i) Preparation of 4-bromo-2,5-difluorobenzoic acid (i-7b)To a solution of l,4-dibromo-2,5-difluorobenzene (i-7a) (1.1 g , 4 mmol) in Et20 (10 mL) at – 78 C was added n-BuLi (2.5M in hexane, 1.6 mL, 4 mmol) dropwise. The mixture was stirred for 30 min at -78 C and then quenched with an excess of freshly crushed dry ice. After 15 min, the mixture was brought to rt and diluted with H20. The aqueous layer was separated, and the organic layer was extracted with 10% aq. Na2C03. The combined aqueous layers were acidified with 1M HC1 and extracted with EtOAc. The combined organic layers were dried with Na2S04 and concentrated to give the title compound. LCMS (ESI) calc’d for C7H3BrF202 [M+H]+: 237, found: 237

The synthetic route of 327-51-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; MERCK SHARP & DOHME CORP.; N.V. ORGANON; KARSTENS, Willem Frederik Johan; STELT, Mario van der; CALS, Jos; AZEVEDO, Rita Corte Real Goncalves; BARR, Kenneth Jay; ZHANG, Hongjun; BERESIS, Richard Thomas; ZHANG, Dongshan; DUAN, Xiaobang; WO2012/106995; (2012); A1;,
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Electric Literature of 626-39-1, These common heterocyclic compound, 626-39-1, name is 1,3,5-Tribromobenzene, 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.

[0372] 1,3,5-Tribromo-benzene (31.4 g, 100 mmol) was dissolved under argon in a flame dried three-neck flask in 1000 mL diethylether and the solution was cooled to -72C. A solution of 62 mL r°BuLi (1.6 M in hexane, 100 mmol) was added to the resulting suspension in such a fashion that temperature did not rise above -7O0C. The mixture was stirred for 30 min at -750C and the reaction was monitored by HPLC. A solution of 10.4 g (100 mmol) 3-cyanopyridine in 100 mL diethylether was added in such a fashion that temperature did not rise above -710C. The mixture was stirred at -75C for 60 min and the reaction was monitored by HPLC. The cooling bath was removed and warmed to -250C. 2 N HCl (250 mL) was added and the mixture was stirred for 20 min at room temperature. The mixture was made alkaline by addition of 1 N NaOH. The product was extracted with ethyl acetate and the combined organic layers were dried over Na2SO4. The product was purified by chromatography (700 g silica agel, CH2Cl2, then CH2Cl2 / ethyl acetate 1:1, UV) to yield 27.7 g (81 %) of (3,5-dibromo-rhohenyl)-pyridin-3-yl-methanone.

The synthetic route of 626-39-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; LOCUS PHARMACEUTICALS, INC.; WO2008/8059; (2008); A1;,
Bromide – Wikipedia,
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Adding a certain compound to certain chemical reactions, such as: 626-88-0, name is 1-Bromo-4-methylpentane, 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 626-88-0, Recommanded Product: 626-88-0

To a solution of 7-(3,4-dimethoxybenzyl)-4-chloro-5H-pyrrolo[3,2-d]pyrimidin-2- amine (227 mg, 0.71 mmol, 1.00 equiv) in DMF (50 mL) was added l-bromo-4- methylpentane (141 mg, 0.85 mmol) and then NaH (34 mg, 1.42 mmol). The resulting solution was stirred for 4 hours at room temperature. The reaction was then quenched by the adding 50 mL of H2O/ice. The resulting solution was extracted with 3 x 50 mL of EtOAc. The organic layers were combined, dried over Na2SO4, and concentrated under vacuum using a rotary evaporator. The residue was purified by recrystallization from EA : hexane (1 : 5), resulted in 39 mg (14%) of 7-(3,4-dimethoxybenzyl)-4-chloro-5-(4-methylpentyi)-5H- pyrrolo[3,2-d]pyrimidin-2-amine as a yellow solid. 1H NMR (300 MHz, CDCl3) delta 0.86 (6H, s), 1.15 (2H, m), 1.61 (IH, m), 1.75 (2H, m), 3.85 (6H, s), 3.95 (2H, s), 4.19 (2H, s), 4.87 (2H, s), 6.80-6.89 (4H, m). MS m/z: 403 [M+l] + .

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

Reference:
Patent; PONIARD PHARMACEUTICALS, INC.; WO2009/139834; (2009); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Reference of 129316-09-2, The chemical industry reduces the impact on the environment during synthesis 129316-09-2, name is 1,3-Dibromo-5-(tert-butyl)benzene, I believe this compound will play a more active role in future production and life.

Synthesis of intermediate 4-(biphenyl-4-yl)-1-(3-bromo-5-tert-butylphenyl)-1H-imidazole 13 4-(Biphenyl-4-yl)-1H-imidazole 12 (3773 mg, 17.13 mmol, 1.0 eq), CuI (326 mg, 1.71 mmol, 0.1 eq), L-proline (394 mg, 3.42 mmol, 0.2 eq), 1,3-dibromo-5-(1,1-dimethylethyl)-benzene (8.00 g, 27.40 mmol, 1.6 eq) and K2CO3 (4735 mg, 34.26 mmol, 2.0 eq) were added to a dry pressure tube equipped with a magnetic stir bar. The vissel was then evacuated and backfilled with nitrogen, this evacuation and backfill procedure was repeated for a total of three times. Then DMSO (35 mL) were added in a nitrogen filled glove box. The mixture was bubbled with nitrogen for 5 minutes. The tube was sealed before being taken out of the glove box. The mixture was stirred in an oil bath at a temperature of 105-115 C. for 3 days. Then the mixture was cooled to ambient temperature, filtered and washed with a plenty of ethyl acetate. The filtrate was washed with water three times, dried over sodium sulfate, filtered, concentrated under reduced pressure and the residue was purified through column chromatography on silica gel using hexane and ethyl acetate (10:1-5:1-3:1) as eluent to obtain the desired product 13 as a brown-red solid 2.023 g in 26% total yield for the two steps. 1H NMR (DMSO-d6, 400 MHz): delta 1.37 (s, 9H), 7.38 (t, J=7.2 Hz, 1H), 7.49 (t, J=8.0 Hz, 2H), 7.55 (d, J=1.6 Hz, 1H), 7.32-7.75 (m, 5H), 7.88 (d, J=1.2 Hz, 1H), 7.98 (d, J=8.4 Hz, 2H), 8.49 (s, 2H).

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-(tert-butyl)benzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Li, Jian; Li, Guijie; US2015/194616; (2015); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Synthetic Route of 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.

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.

The synthetic route of 583-75-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Ligand Pharmaceuticals Incorporated; US5693647; (1997); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Some common heterocyclic compound, 656-64-4, name is 3-Bromo-4-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. COA of Formula: C6H5BrFN

Benzoyl chloride (18.5 g, 132 mmol) was added to a solution of ammonium thiocyanate (12 g, 158 mmol) in acetone (350 mL) over 5 minutes and the mixture was refluxed for 15 minutes. 3-Bromo-4-fluoroaniline (25 g, 132 mmol) was added to the mixture at 40 and refluxing was continued for 30 minutes. The hot solution was poured over ice (400 mL) and the mixture was stirred for 5 minutes until a precipitate formed, which was collected by filtration and washed with 50% methanol in water (50 mL). To the precipitate was added a 5% sodium hydroxide solution (1000 mL) and the suspension was stirred for 2 hours at 60*0. The mixture was ai lowed to cool down to room temperature and stored at room temperature for 3 days while a precipitate formed, which was collected by filtration, washed with water and dried under reduced pressure to yield 22.2 g (67%) 1-(3-bromo-4-fluorophenyl)thiourea1 H-NMR (300 MHz, DMSO-cfe) delta = 7.34 (dd, 1 H), 7.35 (ddd, 1 H), 7.59 (br, 2H), 7.85 (dd, 1 H) 9.75 (br, 1 H) ppm.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 656-64-4, its application will become more common.

Reference:
Patent; BAYER PHARMA AKTIENGESELLSCHAFT; ROeHN, Ulrike; SCHMITT-WILLICH, Heribert; HEINRICH, Tobias; BERGER, Markus; FITZNER, Ansgar; KRAUSE, Sabine; BROCKSCHNIEDER, Damian; DYRKS, Thomas; THIELE, Andrea; MOeNNING, Ursula; BOeMER, Ulf; WO2012/7510; (2012); A1;,
Bromide – Wikipedia,
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Related Products of 1074-24-4,Some common heterocyclic compound, 1074-24-4, name is 1,4-Dibromo-2,5-dimethylbenzene, molecular formula is C8H8Br2, 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.

1,4-dibromo-2,5-dimethylbenzene: 1H-1,2,4- triazole: potassium carbonate: copper oxide molar ratio is 2: 10: 30: 1. To a 50mL three-neck round bottom flask equipped with a magnetic stirrer, reflux condenser and thermometer was added CuO (0.0398mg,0.5mmol), potassium carbonate (2.0731g, 15mmol), 1H-1,2,4-triazole (0.345mg, 5mmol), 1,4- dibromo-2,5-dimethylbenzene (0.3360g, 1mmol ), 20mL DMF. Stirring at 100 deg.C. React for 24 hours. After completion of the reaction, the reaction solution was cooled to room temperature, filtered and the filtrate was added 100mL of water, heavy precipitate precipitation, filtration, filter cake was collected, yield 60percent.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1,4-Dibromo-2,5-dimethylbenzene, its application will become more common.

Reference:
Patent; Tianjin Normal University; Wang, Ying; (11 pag.)CN105669720; (2016); A;,
Bromide – Wikipedia,
bromide – Wiktionary