Bromides-buliding-blocks

Reference of 69321-60-4, 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. 69321-60-4, name is 2,6-Dibromotoluene, This compound has unique chemical properties. The synthetic route is as follows.

A mixture of 1,3-dibromo-2-methylbenzene (Combi Blocks catOT-1437: 339 mg, 1.356 mmol), tert-butyl 2-(2-methyl-3-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)phenyl)-4,6-dihydro-5H-pyrrolo[3,4-d]thiazole-5-carboxylate (200.0 mg, 0.452 mmol), sodium carbonate (96 mg, 0.904 mmol) and tetrakis(triphenylphosphine)palladium(0) (52.2 mg, 0.045 mmol) in dioxane (3.00 mL)/ water (1.0 mL) was heated at 90 C. overnight. The reaction was then cooled to room temperature, diluted with saturated aqueous NH4Cl, and extracted with EtOAc (3¡Á30 mL). The combined organic layers were washed with brine, dried over Na2SO4, filtered, and the filtrate was concentrated under reduced pressure. The crude residue was purified by chromatography on silica gel, eluting with 0-40% EtOAc/hexanes, to give the desired product (210 mg). LC-MS calculated for C24H26BrN2O2S (M+H)+: m/z=485.1/487.1; found 485.0/487.0.

The chemical industry reduces the impact on the environment during synthesis 2,6-Dibromotoluene. I believe this compound will play a more active role in future production and life.

Reference:
Patent; Incyte Corporation; Wu, Liangxing; Qian, Ding-Quan; Lu, Liang; Lajkiewicz, Neil; Konkol, Leah C.; Li, Zhenwu; Zhang, Fenglei; Li, Jingwei; Wang, Haisheng; Xu, Meizhong; Xiao, Kaijiong; Yao, Wenqing; (101 pag.)US2018/177784; (2018); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

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. 2789-89-1, name is 1,2-Bis(4-bromophenyl)ethyne, A new synthetic method of this compound is introduced below., HPLC of Formula: C14H8Br2

To a 13 ¡Á 150 mm test tube equipped with magnetic stir bar were added [RhCp*(CH3CN)3](SbF6)2 (6.6mg, 4 mol %), NaOAc (32.8mg, 0.4 mmol, 2 equiv) and 2a-2o (0.3 mmol, 1.5 equiv). The test tube was sealed with a rubber septum and removed from the glove-box. The solution of 1a-1r (0.2 mmol, 1 equiv)in EtOH (2 mL) was injected into the test tube via syringe. The reaction mixture was placed in a preheated oil bath (60 ) for 12 h. Then the reaction mixture was concentrated in vacuo, the residue was dissolved in methylene chloride and purified by column chromatography (silica gel, n-hexane/EtOAc =20/1). 1-Methyl-3,4-diphenylisoquinoline (3aa): The title compound was obtained as white crystal in 91% yield (54.2 mg). 1H NMR (400 MHz, CDCl3) delta 8.24 – 8.16(m, 1H), 7.66 (m, 1H), 7.63 – 7.55 (m, 2H), 7.41 – 7.28 (m, 5H), 7.26 – 7.12 (m,5H), 3.09 (s, 3H). 13C NMR (101 MHz, CDCl3) delta 157.78, 149.37, 140.90, 137.56,136.06, 131.44, 130.32, 130.04, 129.29, 128.24, 127.66, 127.18, 127.01, 126.62,126.29, 126.19, 125.60, 22.73. HRMS (EI) calcd. for C22H17N: [M]+, 295.1361. Found: m/z 295.1358.

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; Chu, Benfa; Fang, Lili; Guo, Shan; Qi, Bing; Shi, Pengfei; Wang, Qi; Zhu, Jin; Tetrahedron Letters; (2020);,
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Application of 67567-26-4, 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 67567-26-4 as follows.

To 4-bromo-2,6-difluoroaniline (1.0 g, 4.81 mmol) and copper (I) cyanide (1.28 g, 14.3 mmol) was added DMF (10 mL) under nitrogen and the resulting mixture was heated at 160 C for 18 h. After 18 h, the mixture was cooled, poured onto a 12% aqueous ammonia solution and extracted with EtOAc (2X). The combined organic extract was washed with water. The organic phase was combined with a little water and was filtered through celite to remove suspended solids. The organic phase was then separated from the water, then washed with brine, dried over anhydrous sodium sulfate and concentrated under reduced pressure. Purification by flash chromatography (12% EtOAc/ hexanes eluent) provided 4-amino-3,5-difluorobenzonitrile as a white solid. 1H NMR (300 MHz, Chloroform-d) delta 7.19 – 7.14 (m, 2H), 4.29 (br. s, 2H).

According to the analysis of related databases, 67567-26-4, the application of this compound in the production field has become more and more popular.

Reference:
Patent; UNIVERSITY OF HAWAII; TURKSON, James; YUE, Peibin; TIUS, Marcus; BROTHERTON-PLEISS, Christine; LOPEZ TAPIA, Francisco, Javier; (420 pag.)WO2018/136935; (2018); A1;,
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Related Products of 51437-00-4, 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. 51437-00-4, name is 4-Bromo-1-fluoro-2-methylbenzene belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

4-Bromo-2-bromomethyI-l-fluoro-benzene (TJA01131) C7H5Br2F MW 267.92. 5-bromo-2-fluorotoluene (5.00 g, 26.5 mmol), N-bromosuccinimide (5.18 g, 29.1 mmol), benzyl peroxide (0.205 gs 0.850 mmol) and carbon tetrachloride (50 mL) were loaded to a -r.b. flask and set to reflux (79 0C) for 2 h. Once cooled the succinimide was filtered off and carbon tetrachloride removed via a dry ice-acetone cooled rotary evaporator. The residues were dissolved in dichloromethane (100 mL) and washed with distilled H2O (50 mL x 3) and brine (50 mL). Dried over MgSO4 and solvent removed in vacuo to yield the title compound as a colourless liquid yellow (6.80 g, 96 %), R/. 0.55 (dichloromethane/hexane 10:90), c.f. 0.79 (5-bromo-2-fluorotoluene); HPLC (70 % CH3CN in H2O) tr=4.786 (71.55 %).

The synthetic route of 4-Bromo-1-fluoro-2-methylbenzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; STERIX LIMITED; WO2007/68905; (2007); A1;,
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Adding a certain compound to certain chemical reactions, such as: 955959-84-9, name is 4-(4-Bromophenyl)dibenzo[b,d]furan, 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 955959-84-9, HPLC of Formula: C18H11BrO

Intermediate M-1 in a round bottom flask 10.0g (30.9mmol) and M-32 15.5g (30.9mmol),Sodi um-t- butoxide placed 4.46g (46.35mmol) was dissolved was added to 155ml of toluene. Here Pd2 (dba) 3 0.28g (0.31mmol) and tri-tert-butylphosphine was placed to 0.18g (0.93mmol) in turn and the mixture was stirred under reflux for 12 hours under a nitrogen atmosphere. After the reaction extracted with distilled water and toluene and the organic layer was dried with magnesium sulfate, filtered and the filtrate was concentrated under reduced pressure. The product n- hexane / dichloromethane (8: 2 by volume) to yield the silica gel column chromatography to give compound 9 as 20.71g (90percent yield).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 4-(4-Bromophenyl)dibenzo[b,d]furan, and friends who are interested can also refer to it.

Reference:
Patent; SAMSUNG SDI CO., LTD.; JANG, YU NA; HONG, JIN SEOK; KIM, YOUNG KWON; YU, EUN SUN; KIM, CHANG WOO; KIM, HUN; MIN, SOO HYUN; CHO, PYEONG SEOK; (38 pag.)KR2016/12846; (2016); A;,
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Application of 6138-90-5,Some common heterocyclic compound, 6138-90-5, name is Geranyl bromide, molecular formula is C10H17Br, 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 26(4E)-2-(4-Methoxy-benzenesulfonyl)-5,9-dimethyl-2-[4-(2-morpholin-4-yl-ethoxy) – benzyl]-deca-4,8-dienoic acid hydroxyamide To a stirred solution of (4-methoxy-benzenesulfonyl)-acetic acid ethyl ester (5.16 g, 20 mmol), geranyl bromide (4.2g, 20 mmol) and 18-Crown-6 (500 mg) in acetone (250 ml) was added K2CO3 (10 gms, excess) and the mixture refluxed foe 24 hours. At the end, the reaction mixture was filtered and the acetone layer was concentrated. The residue obtained was extracted with chloroform, washed well with water, dried over anhydrous MgSO4, filtered and concentrated. The product obtained was purified by silica-gel column chromatography, eluting with 30% ethy acetate: hexane. The product 2-(4-methoxy-benzenesulfonyl)-5,9-dimethyl-deca-4,8-dienoic acid ethyl ester was isolated as a colourless oil. Yield: 7.0 g, 89%.

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

Reference:
Patent; Wyeth Holdings Corporation; EP970046; (2003); B1;,
Bromide – Wikipedia,
bromide – Wiktionary

Related Products of 3344-70-5,Some common heterocyclic compound, 3344-70-5, name is 1,12-Dibromododecane, molecular formula is C12H24Br2, 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.

1.0 g of compound 3,2.63 g of 1,12-dibromododecane,0.43 g of potassium hydroxide and 0.16 g of tetrabutylammonium bromide,Was added to a mixture of 10 ml of dichloromethane and 6.5 ml of water,The mixture was stirred at room temperature under nitrogen for 24 hours,With 30 millilitersWashed twice with water, washed once with 15 ml of saturated brine, the organic layer was separated, dried over anhydrous sodium sulfate,The solvent was removed on a rotary evaporator and purified by chromatography on a 200-300 mesh silica gel column (eluent ethyl acetate / petroleum ether volume ratio1: 30-1: 10) to give 1.19 g of compound 4 as a pale yellow liquid in 90percent yield.

The synthetic route of 3344-70-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Guilin University of Technology; Kong, Xiangfei; Dai, Shengping; Yang, Willow; Deng, Sea; Wang, Guixia; (8 pag.)CN106117224; (2016); A;,
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. 33884-43-4, name is 2-(2-Bromoethyl)-1,3-dioxane, This compound has unique chemical properties. The synthetic route is as follows., SDS of cas: 33884-43-4

Synthesis Example 9 Synthesis of 3-(1,3-Dioxan-2-yl)-1-(5-norbornen-2-yl)-1-propanol (Monomer 9) A Grignard reagent was customarily prepared from 36.2 g of 2-(2-bromoethyl)-1,3-dioxane in 200 ml of dry tetrahydrofuran. Then 19.5 g of 5-norbornene-2-carbaldehyde was added dropwise over 30 minutes to the Grignard reagent at 20 C. Stirring was continued for 30 minutes whereupon the reaction solution was added to a saturated aqueous solution of ammonium chloride to stop reaction. After diethyl ether extraction, the organic layer was successively washed with water, saturated sodium bicarbonate water and saturated sodium chloride water, dried over anhydrous sodium sulfate, and concentrated in vacuum. It was further purified by vacuum distillation, obtaining 36.2 g of 3-(1,3-dioxan-2-yl)-1-(5-norbornen-2-yl)-1-propanol (boiling point 125 C./27 Pa, yield 95%). IR (thin film): nu=3440 (br.), 3056, 2962, 2860, 2731, 2657, 1570, 1448, 1404, 1377, 1336, 1284, 1240, 1146, 1093, 1047, 997, 926, 721 cm-1; 1H-NMR (300 MHz in CDCl3): delta=0.45-2.35 (12H, m), 2.55-3.50 (3H, m), 3.65-3.80 (2H, m), 4.05-4.15 (2H, m), 4.40-4.60 (1H, m), 5.80-6.20 (2H, m).

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 33884-43-4.

Reference:
Patent; Shin-Etsu Chemical Co., Ltd.; US6515149; (2003); B2;,
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. 615-36-1, name is 2-Bromoaniline, This compound has unique chemical properties. The synthetic route is as follows., Safety of 2-Bromoaniline

In a 250 mL round bottom flask, 4.0 g (23.3 mmol) of 2-bromoaniline, 16.1 g (116.5 mmol) of anhydrous potassium carbonate, 7.3 mL (116.5 mmol) of methyl iodide (CH3I) and 50 mL of acetonitrile (MeCN) were added and heated. Up to 70 C.After stirring at 70 C for 18 h, the reaction mixture was cooled to room temperature.It was extracted with 100 mL of deionized water and 100 mL of diethyl ether. After the organic phase is separated,The aqueous phase was washed with 3 x 50 mL diethyl ether. The combined organic phase was washed with 5 x 50 mL of saturated brine.The organic phase was then dried over anhydrous magnesium sulfate. Next, the volatile component in the organic phase was distilled off under reduced pressure to give a crude material. The crude product was separated by silica gel column chromatography to yield 2.7 g of pale yellow oily liquid.The eluent was diethyl ether / hexane (5 / 95 v / v), yield 69%. Relevant characterization data is consistent with the literature reported above.

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 615-36-1.

Reference:
Patent; Hubei University; Liu Li; Chen Bulin; (14 pag.)CN108586536; (2018); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Synthetic Route of 1435-51-4, These common heterocyclic compound, 1435-51-4, name is 1,3-Dibromo-5-fluorobenzene, 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.

According to the reaction formula (2), the specific steps are: in a nitrogen atmosphere,Tris (dibenzylideneacetone) dipalladium (0.4mmol), tri-tert-butylphosphorus (1.2mmol),1-Fluoro-3,5-dibromobenzene (10 mmol) and diphenylamine (22 mmol) were dispersed in anhydrous toluene (80 mL), heated to reflux (110 C.) and reacted at this temperature for 16 h. After the reaction system is cooled to room temperature, the reaction solution is diluted, and the diluted reaction solution is suction-filtered with a Buchner funnel covered with silica gel, and the solution is concentrated at a low pressure, and then a mixture of dichloromethane and n-hexane is used in a volume ratio of 1: 1. Silica gel column chromatography was performed as the eluent to obtain di-tertiary amine compound 1a in a yield of 94%.

The synthetic route of 1435-51-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Beijing University Shenzhen Sheng Yuan; Meng Hong; Shi Ming; Sun Yue; (24 pag.)CN110790782; (2020); A;,
Bromide – Wikipedia,
bromide – Wiktionary