Month: June 2021

Adding a certain compound to certain chemical reactions, such as: 57946-63-1, name is 2-Bromo-4-(trifluoromethyl)aniline, 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 57946-63-1, HPLC of Formula: C7H5BrF3N

Example 139 Synthesis of 5- [Acetyl- (3, 5-bis-trifluoromethyl-benzyl)-amino]-7-trifluoromethyl-2, 3,4, 5- tetrahydro-benzo [b] azepine-1-carboxylic acid tert-butyl ester. Step 1. Preparation of Methyl-3-trifluoromethyl-2-aminobenzoate Add palladium (II) acetate (1.89 g, 8.4 mmol), 1,1- bis (diphenylphosphino) ferrocene (6.83 g, 12.3 mmol), and triethyl amine (32 mL, 44.0 mmol) to a solution of 2-bromo-4-trifluoromethylanaline (10.0 g, 42.0 mmol) in dimethylsulfoxide (283 mL) and methanol (187 mL). At 100 psi of carbon monoxide, heat the mixture to 80 °C. After heating for 14-16 h cool the reaction to room temperature and filter. Dilute the organics with ethyl acetate (500 mL), wash with water (3×200 mL) and brine (200 mL). Dry the organics over sodium sulfate and filter. Remove solvent under vacuum and chromatograph the crude product using ethyl acetate/hexane (10 percent) to elute. This provides the title compound (8.0 g, 88percent) as an off white solid: H NMR (CDC13,400 MHz) 8 3.93 (s, 3H), 6.11 (bs, 2H), 6.73 (d, J = 8.4 Hz, 1H), 7.49 (dd, J = 2.0, 8.4 Hz, 1H), 8.17 (d, J = 2.0 Hz, 1H).

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

Reference:
Patent; ELI LILLY AND COMPANY; WO2005/37796; (2005); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Adding a certain compound to certain chemical reactions, such as: 1073-06-9, name is 1-Bromo-3-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 1073-06-9, HPLC of Formula: C6H4BrF

General procedure: In a typical run, a 5-mL vial equipped with a magnetic stirrer was charged with a mixture of phenyl bromide(78.5 mg, 0.5 mmol), styrene (62.5 mg, 0.6 mmol), Pd catalyst (0.0025 mmol), K3PO4 (212 mg, 1.0 mmol) and DMF (1 mL) under nitrogen. The mixture was heated at 100 C for 4 h and then cooled to room temperature. Brine was added, and the resulting mixture was extracted with ethyl acetate (3 x 5 mL). The GC-MS samples were prepared by diluting 10 lL of ethyl acetate solution to1 mL.

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

Reference:
Article; Du, Yufeng; Liang, Beibei; Yang, Fenglei; Shi, Yanhui; Li, Xiuling; Pang, Guangsheng; Cao, Changsheng; Transition Metal Chemistry; vol. 42; 3; (2017); p. 193 – 201;,
Bromide – Wikipedia,
bromide – Wiktionary

Application of 138526-69-9,Some common heterocyclic compound, 138526-69-9, name is 1-Bromo-3,4,5-trifluorobenzene, molecular formula is C6H2BrF3, 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.

General procedure: A mixture of the styrene (3 mmol), the halogenated benzene (3 mmol), triethanolamine (3 mmol) and Pd(II) acetate (0.03 g) was stirred under argon at 100 C for 24 h. The reaction was cooled to 25 C, quenched by the addition of dil. aq. hydrochloric acid (2 N, 10 ml), and extracted with ether (3 × 100 ml). The organic phases were dried (Na2SO4), the solvents evaporated, and the crude product subjected to chromatography (silica gel, hexane/ethyl acetate mixtures).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1-Bromo-3,4,5-trifluorobenzene, its application will become more common.

Reference:
Article; Albert, Sabrina; Horbach, Ralf; Deising, Holger B.; Siewert, Bianka; Csuk, Rene; Bioorganic and Medicinal Chemistry; vol. 19; 17; (2011); p. 5155 – 5166;,
Bromide – Wikipedia,
bromide – Wiktionary

Some common heterocyclic compound, 2924-09-6, name is 5-Bromo-2-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. Product Details of 2924-09-6

To a solution of 5-bromo-2-fluoroaniline (5 g, 26.3 mmol) in DMF (30 mL) was added NCS (3.69 g, 27.6 mmol).The mixture was stirred at 60 C for 2 hr. The mixture was diluted with water, extracted with ethyl acetate twice. Then the organic layer was dried over magnesium sulfate, filtered and concentrated in vacuum. The residue was purified by CombiFlash, eluted with ethyl acetate in hexane (0-5%, 40 min), collected the desired fraction to afford the title compound (1 .2 g, 5.35 mmol, 20.32 % yield). 1 H NMR (400 MHz, DMSO-d6) delta 7.03 (dd, J = 10.8, 8.7 Hz, 1 H), 6.90 (dd, J = 8.8, 5.1 Hz, 1 H), 5.77 (s, 2H). LC-MS: [M+H]+ = 223.9,226.0,228.3.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2924-09-6, its application will become more common.

Reference:
Patent; NOVARTIS AG; DU-CUNY, Lei; XIAO, Qitao; XUN, Guoliang; ZHENG, Qiangang; (204 pag.)WO2018/234978; (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. 58971-11-2, name is 3-Bromophenethylamine, A new synthetic method of this compound is introduced below., Safety of 3-Bromophenethylamine

A mixture of 2-(3-bromophenyl)ethanamine (0.7 mL, 4.9 mmol), acetic anhydride (1 mL, 10.6 mmol), triethylamine (1.4 mL, 10.0 mmol) and DCM (25 mL) was stirred at RT or 18 h, diluted with DCM (50 mL) and washed with NaHCO3 (aq. sat.) (50 mL). The organic phase was separated and dried over Na2SO4, filtered reduced in vacuo. The residue was purified by silica column chromatography eluting with 20-100% EtOAc in Pet. Ether to afford N-[2-(3-bromophenyl)ethyl]acetamide (1.19 g, 4.92 mmol, 99% yield). UPLC-MS (ES+, Method A): 1.41 min, m/z 243.9 [M+H]+.

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; REDX PHARMA PLC; JONES, Clifford, D.; BUNYARD, Peter; PITT, Gary; BYRNE, Liam; PESNOT, Thomas; GUISOT, Nicolas, E.S.; (318 pag.)WO2019/145729; (2019); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Reference of 3344-70-5, These common heterocyclic compound, 3344-70-5, name is 1,12-Dibromododecane, 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.

Phenothiazine and 1,12-dibromododecane (molar ratio = 1:10), potassium hydroxide and DMSO were added to a three-necked flask, filledwith nitrogen, and stirred at room temperature for 12 hours. The reaction mixture was washed with water and extracted with dichloromethane. , Drying over anhydrous, vortexing, andsilica gel column chromatographywith petroleum ether aseluent to give a colorless liquid in a yield of 76.5percent.

Statistics shows that 1,12-Dibromododecane is playing an increasingly important role. we look forward to future research findings about 3344-70-5.

Reference:
Patent; Jiangxi Agricultural University; Hong Yanping; Jiang Yan; Yin Xiaoli; Wu Guoqiang; Liao Xiaoning; Wang Chunrong; Li Liyu; (27 pag.)CN107698999; (2018); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Synthetic Route of 1347736-74-6, 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. 1347736-74-6, name is 4,7-Dibromo-5-fluoro-2,1,3-benzothiadiazole belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

the 4,6-dibromo-5-fluorobenzo [c] [1, 2, 5] thiadiazole (2.00g, 6 . 41 mmol) and ethanol (50 ml) is added to the three-hole and round-bottom flask cooled to 0 C. In slowly adding Na[BH4] (4.6g, 0 . 12 mol) later, the reaction mixture is stirred at room temperature overnight. After removing the volatile substance, the 100 distilled water added to the reaction mixture, then the mixture is extracted with ethyl ether, salt water cleaning, and the anhydrous Na2SO4dry. Removing volatile substances from the extract to obtain a light brown powder A (1.20g, 66%).

The synthetic route of 4,7-Dibromo-5-fluoro-2,1,3-benzothiadiazole has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SABIC Global Technology Company; Ibrahim Lafia, S·M·; Tate, C. Haug; Gillian, M · Bristol Senanayake; Amit, K · Jiefudiya; Ahmed, I. Abdul Rahman; (26 pag.)CN105531280; (2016); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Reference of 103-64-0,Some common heterocyclic compound, 103-64-0, name is (2-Bromovinyl)benzene, molecular formula is C8H7Br, 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.

General procedure: A mixture of thiophenols (0.5 mmol), 1-((E)-2-iodovinyl)benzenes (0.6 mmol), CuI (19 mg, 20 mol %), L5 (19 mg, 20 mol %), and Cs2CO3 (326 mg, 2 equiv) in DMSO (3 mL) was stirred in N2 at 100 C for 24 h., The mixture was quenched with saturated salt water (10 mL) after the reaction completion. The solution was extracted with ethyl acetate (3×10 mL). The organic layers were combined and dried by sodium sulfate. The product 2-(styrylthio)phenols was obtained by flash column chromatography on silica gel.

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

Reference:
Article; Xu, Run-Sheng; Yue, Lei; Pan, Yuan-Jiang; Tetrahedron; vol. 68; 25; (2012); p. 5046 – 5052;,
Bromide – Wikipedia,
bromide – Wiktionary

Adding a certain compound to certain chemical reactions, such as: 59907-12-9, name is 1-Bromo-2-fluoro-3-methylbenzene, 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 59907-12-9, Formula: C7H6BrF

General procedure: To an oven-dried 25 mL Schlenk tube containing a stirring bar was added 4.5 mg Pd(OAc)2 (0.02 mmol), 15.7mg nBuPAd2 (0.44 mmol), 2-bromofluorobenzene (0.50 mmol), salicylaldehyde (0.50 mmol), potassium carbonate (1.0 mmol). The Schlenk tube was vacuumed and then purged with argon before DMF (2.0 mL) was injected using a syringe. Afterwards the Schlenk tube in the ice bath was degassed by evacuation and back fillingwith argon three times. The reaction mixture was then stirred for 12 h at 120 C. After the reaction was complete,the reaction mixture was diluted with water (5 mL), extracted with ethyl acetate (3 x 10 mL) and dried withanhydrous Na2SO4. After filtration and addition of silica gel into the solution, the organic solvent was reduced evaporated. The crude product was purified by column chromatography using ethyl acetate/n-pentane.

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-2-fluoro-3-methylbenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Shen, Chaoren; Wu, Xiao-Feng; Synlett; vol. 27; 8; (2016); p. 1269 – 1273;,
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. 74586-53-1, name is 3-Bromo-5-methylaniline, This compound has unique chemical properties. The synthetic route is as follows., COA of Formula: C7H8BrN

To a solution of 3-bromo-5-nitrotoluene (1500g) in glacial acetic acid (11 I) in a nitrogen purged hydrogenation vessel was added 5% platinum on carbon (approx 50% water wet paste) and the mixture was hydrogenated under 4 bar hydrogen pressure at room temperature. On completion of hydrogen uptake the catalyst was removed by filtration and the filtrate split into two equal portions. Each portion was set to stir separately and a solution of potassium cyanate (500g) in water (1.25 I) was added to each over 15 min. After stirring for an additional 15 min water (10 I) was added and the precipitated solid isolated by filtration and washed with water. The water wet cakes were combined and dissolved in hot EtOAc (3 I) and the aqueous phase separated. The organic phase was cooled with stirring to crystallise the product, which was isolated by filtration and washed with fresh EtOAc (2 I) and air dried overnight. Recrystallisation from ETOH (2. 7 I) afforded the title compound. (565G) LC RT=3.9 mins.

According to the analysis of related databases, 74586-53-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; GLAXO GROUP LIMITED; WO2004/39766; (2004); A1;,
Bromide – Wikipedia,
bromide – Wiktionary