Author: Jessica.F

Reference of 268733-18-2, 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. 268733-18-2, name is 4-Bromo-3,5-bis(trifluoromethyl)aniline belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Disodium phosphate 18.2 g (123 mmol) and tetrabutylammonium hydrogen sulfate 2.1 g (6.20 mmol) were dissolved in a 500 mL solution of acetone and dichloromethane, followed by the addition of 4-bromo-3,5-bis-trifluoromethyl aniline 10.0 g (32.5 mmol) dropwise with a oxone and the reaction solution was stirred for 1 hour at 0 C. Potassium hydroxide was added to maintain the acidity of the reaction solution between 7.5 and 8.5. After completion of the reaction, the solution was diluted with dichloromethane and washed with distilled water several times to remove salts. Magnesium sulfate was then added to the dichloromethane solution and the solvent was filtered then evaporated and the resulting reactant was passed through a silica column pale to give a light yellow compound, 1-bromo-4-nitro-2,6-bis(trifluoromethyl)benzene (8.05 g, 23.8 mmol 73.3% yield). [0103] Melting point: 56-57 C. [0104] 1H NMR (CDCl3, 400 MHz, ppm): 8.71 (s, 2H). [0105] 13C NMR (DMSO-d6, 100 MHz, ppm): 146.62, 132.48 (q, J=31.9 Hz), 126.71 (q, J=5.7 Hz), 125.63, 121.68 (q, J=272.9 Hz).

The synthetic route of 4-Bromo-3,5-bis(trifluoromethyl)aniline has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Kim, Sang Youl; Kim, Sun Dal; Chung, Im Sik; US2015/45481; (2015); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Electric Literature of 1786-36-3, 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. 1786-36-3, name is (2-Bromo-1-fluoroethyl)benzene belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Under a nitrogen atmosphere, nickel bromide (4.4 mg, 0.02 mmol),4,4′-dimethyl-2,2′-bipyridine (3.68 mg, 0.02 mmol),Tetrabutylammonium iodide (14.77 mg, 0.04 mmol) manganese powder (43.95 mg, 0.8 mmol),Add solvent NMP (0.5 mL) and stir well. Weigh 4-bromoacetophenone (39.81mg, 0.2mmol) in NMP (0.5mL),After dissolution, add (2-bromo-1-fluoroethyl) benzene (60.92 mg, 0.3 mmol) and mix well.The solution was transferred to a sealed tube. After sealing, the reaction was stirred in an oil bath at 80 C for 24 hours.Cool the reaction to room temperature, ether (5mL)Add an equal volume of saturated ammonium chloride solution to the diluted reaction solution.Filter through a diatomaceous sand core funnel, rinse with a small amount of ether, and collect the filtrate.The filtrate was extracted three times with diethyl ether, and the organic phases were combined (add internal standard dodecane,GC-MS determined crude yield). Dried over anhydrous sodium sulfate,Filtration, distillation to remove the solvent under reduced pressure,After the residue was separated by silica gel column chromatography, the product was weighed.The calculated yield was 39%.

The synthetic route of (2-Bromo-1-fluoroethyl)benzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Sichuan Qing Chemical University; Yang Yi; Luo Gen; Li Youlin; Tong Xia; He Mengmeng; Jiang Yan; Liu Yingle; Shu Yumei; Zheng Yubin; Lu Wenjie; Zhao Yanchuan; (22 pag.)CN110803977; (2020); A;,
Bromide – Wikipedia,
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Synthetic Route of 113899-55-1, These common heterocyclic compound, 113899-55-1, name is 1-(2-Bromophenyl)ethylamine, 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.

Add diisopropylethylamine (1.5 g, 12 mmol) to a solution of l-(2-bromo-4- fluoro-phenyl)-ethylamine (4 g, 20 mmol) and di-tert-butyldicarbonate (6.5 g, 30 mmol) in 20 mL of DCM. Stir the mixture overnight at RT. Dilute the mixture with chloroform/IPA (3/1), wash with aqueous saturated sodium chloride and water, dry it over sodium sulfate and concentrate in vacuo. Purify the crude product by column chromatography (10 % methanol in DCM) to give the title compound (2.0 g, 33 %). MS (ES) m/z 244/246 [M-tert-butyl]+.

Statistics shows that 1-(2-Bromophenyl)ethylamine is playing an increasingly important role. we look forward to future research findings about 113899-55-1.

Reference:
Patent; ELI LILLY AND COMPANY; WO2008/144223; (2008); A2;,
Bromide – Wikipedia,
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Application of 18869-30-2,Some common heterocyclic compound, 18869-30-2, name is (E)-1,2-Bis(4-bromophenyl)ethene, molecular formula is C14H10Br2, 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.

A 100 mL three-neck flask was charged with 0.80 g (2.37 mmol) of 4,4′-dibromostilbene synthesized in Step 2, 1.2 g (5.40 mmol) of 9-phenanthrene boronic acid, 0.0053 g (0.024 mmol) of palladium acetate, and 0.050 g (0.163 mmol) of tris(o-tolyl)phosphine, and the air in the flask was replaced by nitrogen. Then, 15 mL of ethylene glycol dimethyl ether and 3.5 mL (2.0 mol/L) of potassium carbonate aqueous solution were added thereto and stirred for 8 hours at 90 C. to cause a reaction. After the reaction, precipitate in the reaction mixture was collected by suction filtration. After the filtration, the obtained material was recrystallized from chloroform and hexane to obtain 0.86 g of white solid in a yield of 68%. The obtained white solid was identified as DPNS2 by a nuclear magnetic resonance method (NMR). 1H-NMR of the obtained DPNS2 is shown below. In addition, a 1H-NMR chart is shown in FIG. 15. 1H-NMR (300 MHz, CDCl3); delta=8.81-8.73 (m, 4H), 8.02-7.91 (m, 4H), 7.74-7.57 (m, 18H), 7.34 (s, 2H) A synthesis scheme of DPNS2 is shown below.; Further, when a decomposition temperature Td of DPNS2 was measured by a thermo-gravimetric/differential thermal analyzer (TG/DTA 320, manufactured by Seiko Instruments Inc.), the Td was 416.6 C . Therefore, it was understood that DPNS2 has a high Td. An absorption spectrum of DPNS2 in a state of being dissolved in a toluene solvent is shown in FIG. 16 and that in a thin film state is shown in FIG. 18. An emission spectrum of DPNS2 in the toluene solution is shown in FIG. 17 and that in the thin film state is shown in FIG. 19. In each of FIGS. 16 and 18, the vertical axis indicates absorption intensity (arbitrary unit) and the horizontal axis indicates wavelength (nm). Also, in each of FIGS. 17 and 19, the vertical axis indicates emission intensity (arbitrary unit) and the horizontal axis indicates wavelength (nm). A light emission from DPNS2 had a peak at 420 nm (an excited wavelength: 348 nm) in the state of DPNS2 being dissolved in the toluene solution and had a peak at 437 nm (an excited wavelength: 344 nm) in a thin film state, therefore, it is understood that blue light emission was obtained. Using absorption spectrum data in FIG. 18, an absorption edge was obtained from a Tauc plot. Then, the energy at the absorption edge is used as an energy gap and an energy gap of DPNS2 was found to be 3.2 eV. Since 9,10-diphenylanthracene, which exhibits representative blue emission, has an energy gap of 2.9 eV, it is understood that DPNS2 has a very large energy gap. Further, the HOMO level in the thin film state was measured by an ambient photoelectron spectroscopy with a spectrometer (AC-2, manufactured by Riken Keiki Co., Ltd.), and was found to be -5.9 eV. Using the HOMO level and the energy gap, the LUMO level was found to be -2.7 eV. An optimal molecular structure of DPNS2 in a ground state was calculated by the same method as Synthesis Example 1. From this calculation result, a HOMO level value of the obtained DPNS2 was found to be -5.59 eV. Singlet excitation energy (energy gap) of DPNS2 was calculated by the same method as Synthesis Example 1. The singlet excitation energy was calculated to be 3.34 eV.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route (E)-1,2-Bis(4-bromophenyl)ethene, its application will become more common.

Reference:
Patent; Semiconductor Energy Laboratory Co., Ltd.; US2007/100180; (2007); 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. 875664-38-3, name is 1-Bromo-4,5-difluoro-2-methylbenzene, A new synthetic method of this compound is introduced below., HPLC of Formula: C7H5BrF2

General procedure: To a solution of o—dibromobenzenes, N—Boc—pyrrole—2—boronic acid 2 and 1.0 M K2CO3aq. in DMF was added PdCl2(PPh3)2 (20%/mol) under a nitrogen atmosphere. Theresulting mixture was heated at 80 C for 7 h. After cooling to room temperature, themixture was extracted with a mixture of EtOAc/hexane (v/v = 1:4). The organic layerwas washed with water and brine, and then dried over Na2SO4. After removal solvent,the residue was purified by silica gel column chromatography and recrystallization todi(N—Boc—pyrrol—2—yl—benzenes).

The synthetic route of 875664-38-3 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Kuzuhara, Daiki; Miyake, Satoshi; Moriyama, Hirotake; Tamura, Yuto; Aratani, Naoki; Yamada, Hiroko; Tetrahedron Letters; vol. 56; 41; (2015); p. 5564 – 5567;,
Bromide – Wikipedia,
bromide – Wiktionary

Adding a certain compound to certain chemical reactions, such as: 627526-90-3, name is 1-Bromo-3-(difluoromethyl)-5-fluorobenzene, 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 627526-90-3, HPLC of Formula: C7H4BrF3

A mixture of 1-bromo-3-(difluoromethyl)-5-fluoro-benzene (ig, 4.44 mmol) and 1- cyclopropylpiperazine (2.80 g, 22.22 mmol) was microwaved at 200 C for 1 h. Pumped down solvent and purified the crude mixture by ISCO purification (40g silica; 0 % to 5% to 30% of MeOH in DCM) to provide 1-[3-bromo-5-(difluoromethyl)phenyl]piperazine (920 mg, 89%). ?H NMR (300 MHz, CD3OD) oe 7.20 (s, 1H), 7.09 (s, 1H), 7.05 (d, J = 1.0 Hz, 1H), 6.66 (t, J = 56.1 Hz, 1H), 3.20 (dd, J = 6.2, 4.0 Hz, 4H), 2.98 (dd, J = 6.2, 4.1 Hz, 4H) ppm. ESI-MS m/z calc. 290.02, found 291.19 (M+1)+; Retention time: 0.63 minutes.

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-(difluoromethyl)-5-fluorobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; VERTEX PHARMACEUTICALS INCORPORATED; DAVIES, Robert, J.; CAO, Jingrong; COCKERILL, Meghan, Elise; COLLIER, Philip, Noel; DENINNO, Michael, Paul; DOYLE, Elisabeth; FRANTZ, James, Daniel; GAO, Huai; GOLDMAN, Brian, Anthony; GREY, Ronald, Lee; GRILLOT, Anne-laure; GU, Wenxin; HENDERSON, James, A.; IRARRAZAVAL, Raul Eduardo, Krauss; KOLPAK, Adrianne, Lynn; LIAO, Yusheng; MAGAVI, Sanjay Shivayogi; MALTAIS, Francois; MESSERSMITH, David; PIERCE, Albert, Charles; PEROLA, Emanuele; RYU, Elizabeth Jin-Sun; SYKEN, Joshua; WANG, Jian; (706 pag.)WO2016/197009; (2016); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Adding a certain compound to certain chemical reactions, such as: 28148-04-1, name is 1,3-Dibromo-2-methylpropane, 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 28148-04-1, Recommanded Product: 1,3-Dibromo-2-methylpropane

The beta- lactam carbonyl compound of the formula shown CH3CH2COCH2CONHC6H51.0mmol added 50 ml round-bottomed flask, followed by adding further Cs2CO32.2mmol, eighteen crown six 0.05mmol, acetic 1.2mmol, 1,3- dibromo – 2-methyl propane 1.15mmol and 35mL of deionized water and mix well. The reaction was continued stirring at 40 deg C 5.0 hours, the reaction was stopped by filtration, dried and purified by recrystallization to give 6-anilino after -5- propionyl-3-methyl-3,4-dihydropyran, products yield 87%.

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

Reference:
Patent; Huaihua University; Xiang, Dexuan; Liang, Chunhua; Liu, Yilin; Xiang, Bailin; Zhang, Li; (9 pag.)CN105541770; (2016); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Electric Literature of 105309-59-9, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 105309-59-9 name is Tetrakis(4-bromophenyl)methane, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

Cz (2.5 g, 8.9 mmol), intermediate TBrBen (2.8 g, 4.5 mmol), CuI (0.19 g, 1.0 mmol) and K3PO4 (1.69 g, 8.0 mmol) were added to 100 mL of toluene.The reaction was carried out under argon gas protection and reflux for 24 hours.After removing the solvent, the residue was extracted with dichloromethane (3×100 mL).The organic phases were combined and dried over anhydrous magnesium sulfate.The residue obtained by concentration was purified by column chromatography using dichloromethane: n-hexane (7:3) as eluent to afford product DCzCBr (2.7 g, yield 50.3%).Identification of intermediates by mass spectrometry,The result is:

At the same time, in my other blogs, there are other synthetic methods of this type of compound, Tetrakis(4-bromophenyl)methane, and friends who are interested can also refer to it.

Reference:
Patent; Yangtze Normal University; Yang Yezi; Yao Chuang; Sun Changqing; (13 pag.)CN108752320; (2018); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Related Products of 1435-54-7, 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. 1435-54-7, name is 1,3-Dibromo-2-fluorobenzene belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Scheme 4-1: In Step 1 the appropriately substituted dibromo species is coupled with an appropriate boronic acid as known in the art to form a mixture of biaryl and triaryl products from which the desired biaryl compound is isolated. In Step 2 the appropriately substituted biaryl species is converted to the Grignard reagent with activated magnesium. In Step 3 the appropriately substituted aldehyde is treated with the previously prepared Grignard reagent to form an alcohol. In Step 4 the appropriately substituted alcohol is converted to a bromide as known in the art with carbon tetrabromide and triphenyl phosphine. In Step 5 the appropriately substituted bromide is converted to the Grignard reagent with activated magnesium.

The synthetic route of 1,3-Dibromo-2-fluorobenzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ACHILLION PHARMACEUTICALS, INC.; WILES, Jason, Allan; PHADKE, Avinash, S.; DESHPANDE, Milind; AGARWAL, Atul; CHEN, Dawei; GADHACHANDA, Venkat, Rao; HASHIMOTO, Akihiro; PAIS, Godwin; WANG, Qiuping; WANG, Xiangzhu; GREENLEE, William; (335 pag.)WO2017/35417; (2017); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Reference of 128259-68-7, These common heterocyclic compound, 128259-68-7, name is 1,3-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.

3-fluorophenol (0.099 mL, 1.1 mmol) and KOH (62 mg, 1.1 mmol) were stirred at 50 °C for 30 min before the addition of l,3-dibromo-2,5-difluorobenzene (300 mg, 1.1 mmol) and Cu powder (70 mg, 1.1 mmol). The reaction mixture was heated to 100 °C overnight. The crude material was purified by FC on silica gel (eluent: Cy), giving l-bromo-2,5-difluoro-3-(3-fluorophenoxy)benzene (P5, 61 mg, y= 18percent) as oil. Eta NMR (METHANOL-rf4): delta ppm 7.49-7.38 (m, 1H), 7.33 (ddd, 1H), 7.02- 6.93 (m, 2H), 6.90-6.82 (m, 2H )

Statistics shows that 1,3-Dibromo-2,5-difluorobenzene is playing an increasingly important role. we look forward to future research findings about 128259-68-7.

Reference:
Patent; SHIRE INTERNATIONAL GMBH; CREMONESI, Susanna; MICHELI, Fabrizio; SEMERARO, Teresa; TARSI, Luca; LUKER, Tim; LESLIE, Colin; (121 pag.)WO2016/42453; (2016); A1;,
Bromide – Wikipedia,
bromide – Wiktionary