Month: September 2021

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. 4101-68-2, name is 1,10-Dibromodecan, A new synthetic method of this compound is introduced below., Quality Control of 1,10-Dibromodecan

Tempol (0.01 mol) was added to a three-neck flask containing 100 ml dry benzene that is maintained at nitrogen atmosphere. To the flask, sodium hydride (0.015 mol) was added and kept refluxed for 24 hrs. The flask was cooled in ice bath and added 1,10-dibromodecane (0.02 mol) in one portion. The refluxing was then resumed for another 72 hrs. The contents of the flask was cooled in ice bath and added 25 ml water and transferred to a separatory funnel. The red upper benzene layer was separated , dried over anhydrous magnesium sulfate and solvent removed by rotory evaporation to get a red oil. The oil was purified by column chromatography on silica gel 60. The material was added to the column and eluted first with about 150 ml hexane that removed the excess of dibromodecane. The desired bromodecanoyl ether of Tempol was eluted with a mixture of hexane and ether (90:10). The red eluate was collected and was found to be pure on thin layer chromatography plates developed using the same solvent mixture. The yield was 0.008 mol (80%).

The synthetic route of 4101-68-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; COLBY PHARMACEUTICAL COMPANY; MEDICAL COLLEGE OF WISCONSIN, INC.; US2011/59922; (2011); 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. 583-70-0, name is 2,4-Dimethylbromobenzene, A new synthetic method of this compound is introduced below., COA of Formula: C8H9Br

General procedure: A flask furnishedwith a dropping funnel was charged with the aryl/alkylbromide in Et2O. n-BuLi(1.6 M in hexane) diluted with Et2O was added dropwise at -78C. After addition, thereaction was kept at -78C for 10 min and was then allowed to warm to room temperatureand stirred for 30 min. The solution was transferred via cannula to SiCl4 dissolved in Et2Oat 0C. The reaction was stirred for 2 h and was allowed to warm to room temperature. Thesolvent was removed under reduced pressure and the residue dissolved in boiling toluene.Insoluble salts were removed via filtration through cellite and washed with hot toluene. Thesolvent from the resulting clear solution was removed under reduced pressure, followed bypurification via distillation or recrystallization.

The synthetic route of 583-70-0 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Binder, Judith; Fischer, Roland C.; Flock, Michaela; Torvisco, Ana; Uhlig, Frank; Phosphorus, Sulfur and Silicon and the Related Elements; vol. 190; 11; (2015); p. 1980 – 1994;,
Bromide – Wikipedia,
bromide – Wiktionary

Synthetic Route of 452-74-4, 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. 452-74-4, name is 1-Bromo-2-fluoro-4-methylbenzene, This compound has unique chemical properties. The synthetic route is as follows.

A degassed solution of 3-amino-furo[3,2-c]pyridine-2-carboxylic acid ethyl ester (300 mg, 1.46 mmol), 4-bromo-3-fluorotoluene (277 mul, 2.19 mmol), Pd2dba3 (67 mg, 0.073 mmol), Xantphos (84 mg, 0.15 mmol) and potassium phosphate tribasic (620 mg, 2.92 mmol) in toluene (10 ml) was heated at reflux under an argon atmosphere for 16 hours. The reaction mixture was concentrated in vacuo and the residue was purified by flash chromatography (Si-SPE, pentane: diethyl ether, gradient 100:0 to 75:25) to afford the title compound as a yellow solid (252 mg, 55%). LCMS (method B): Rx = 3.14 min, M+H+ = 315.

The chemical industry reduces the impact on the environment during synthesis 1-Bromo-2-fluoro-4-methylbenzene. I believe this compound will play a more active role in future production and life.

Reference:
Patent; GENENTECH, INC.; WO2008/24725; (2008); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Reference of 51554-93-9, These common heterocyclic compound, 51554-93-9, name is 1-Bromo-4-octylbenzene, 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 (2.37 g, 11.9 mmol), 1-bromo-4-n-octyl-benzene (4.17 g, 15.4 mmol) and sodium tert-butoxide (2.3 g, 23.8 mmol) are dissolved sufficiently in 50 mL of toluene.Tri tert-butylphosphine(0.144 g, 0.7 mmol)And Pd2 (dba) 3 (0.54 g, 0.59 mmol)After sufficiently dissolving at room temperature under a nitrogen atmosphere,And the mixture is stirred at 120 C under reflux.When the reaction is complete, work-up is carried out with a 1: 1 mixture of water and chloroform.After separating the organic layer after the work-up process using the extraction method,The solvent is removed under reduced pressure.After the solvent was removed, the product was recrystallized several times with methanol to obtain a pale yellow solid product (3.5 g, 76%) was obtained.

The synthetic route of 51554-93-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Daegu Gyeongbuk Institute of Science and Technology Foundation; Jo, Hyo Jung; Kang, Jin Kyu; Nam, Jung Eun; Kim, Dae Hwan; (11 pag.)KR101526327; (2015); B1;,
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, HPLC of Formula: C6H5BrFN

Compound 3 (5 g, 30.9 mmol) was dissolved in 50 mL water and heated to 65 C.Further, Compound 4 (6.5 g, 34.0 mmol) was added, and then a saturated sodium hydrogen carbonate solution (50 mL) was added dropwise.After reacting for 1 hour, it was extracted with ethyl acetate, dried over anhydrous sodiumThe petroleum ether was passed through a column of ethyl acetate (4:1) to afford compound 5 (9 g, 92%) as white solid.

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; Shanghai Xiangjin Biological Technology Co., Ltd.; Sun Fang; Zhan Youni; (38 pag.)CN109574950; (2019); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Synthetic Route of 73918-56-6, These common heterocyclic compound, 73918-56-6, name is 2-(4-Bromophenyl)ethanamine, 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.

General procedure: The appropriate aldehyde 6a-c and 12a-g (1 mmol) was dissolved in 5 mL of CH2Cl2 in a round bottom flask. Then AcOH (1 mmol) and the appropriate amine (1.1 mmol) were added to the stirring solution at room temperature. The mixture was allowed to stir at room temperature for 20 min before NaBH(AcO)3 (3 mmol) was added. The mixture was allowed to stir at room temperature for overnight. Then,after completion, the reaction was quenched with NaOH 1M solution(15 mL). The mixture was then allowed to stir for 30 min. The reaction mixture was then diluted with EtOAc (10 mL), washed two times with EtOAc (10 mL) and once with brine (20 mL). The organic extracts were collected and then dried over Na2SO4, and the solvent was evaporated to yield the crude compounds 7a-e, 13a-o, 14a-b and 15a which were purified by silica gel column chromatography.

Statistics shows that 2-(4-Bromophenyl)ethanamine is playing an increasingly important role. we look forward to future research findings about 73918-56-6.

Reference:
Article; Liu, Pingxian; Yang, Yang; Ju, Yuan; Tang, Yunxiang; Sang, Zitai; Chen, Lijuan; Yang, Tao; An, Qi; Zhang, Tianyu; Luo, Youfu; Bioorganic Chemistry; vol. 80; (2018); p. 422 – 432;,
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. 39478-78-9, name is 5-Bromo-2-methylaniline, A new synthetic method of this compound is introduced below., HPLC of Formula: C7H8BrN

Example 1.Preparation of 2-methyl-5-bromophenylguanidine nitrate of the Formula 3; Preparation of 5-bromo-2-methylaniline hydrochlorideA 5-L reactor has been charged with 812.3 g of 5-bromo-2-methylaniline (4.36 mol. 1.0 eq), and 3.7 kg of methylene chloride. After cooling the obtained clear solution to 1O0C, 190.7 g of dry hydrogen chloride gas was added from a bottle over a period of 2.5 h. The resulting mixture was stirred for ca. 30 minutes, whereafter the obtained crystalline product was filtered off on a filter funnel. The precipitate was washed on a filter funnel with two portions of methylene chloride (200 g each). The product was dried at room temperature for 3 days to yield 976.4 g of 5-bromo-2-methylaniline hydrochloride (100%) having an HPLC purity of 99.6%.

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; TEMAPHARM SP. z o.o.; GRUZA, Henryk; MIREK, Slawomir; JEZEWSKI, Artur; WRZOSEK, Artur; WO2010/14022; (2010); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Related Products of 17247-58-4,Some common heterocyclic compound, 17247-58-4, name is (Bromomethyl)cyclobutane, molecular formula is C5H9Br, 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 stirred solution of the ketimime 1a’ (50 g, 187.1 mmol, available from Aldrich Chemical Company, Milwaukee, Wis.) under N2 in dry THF (400 mL) was cooled to -78 C. and treated with 1 M solution of K-tBuO (220 mL, 1.15 equiv.) in THF. The reaction mixture was warmed to 0 C. and stirred for 1 h and treated with bromomethylcyclobutane (28 mL, 249 mmol). The reaction mixture was stirred at room temperature for 48 h and concentrated in vacuo. The residue was dissolved in Et2O (300 mL) and treated with aq. HCl (2 M, 300 mL) The resulting solution was stirred at room temperature for 5 h and extracted with Et2O (1 L). The aqueous layer was made basic to pH 12-14 with aq. NaOH (50%) and extracted with CH2Cl2 (3×300 mL). The combined organic layers were dried (MgSO4), filtered, and concentrated to give pure amine (1b’, 18 g) as a colorless oil.

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

Reference:
Patent; Schering Corporation; US2006/276405; (2006); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

These common heterocyclic compound, 699-03-6, name is 1-(4-Bromophenyl)-N-methylmethanamine, 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. category: bromides-buliding-blocks

General procedure: Amine (0.25 mmol), and bromide (0.25 mmol) were taken up in acetonitrile (0.3 mL) in a conical vial equipped with a stirrer bar. Potassium carbonate (0.5 mmol) was added followed by potassium iodide (10 mol%) if required. The vial was sealed with a screwcap and the reaction was stirred at 40 C until thin layer chromatography (TLC) indicated complete consumption of the starting materials. A precipitate was formed during the reaction which was removed by filtration and the filtrate concentrated under reduced pressure. The residue was purified by flash column chromatography and sent to the Netherlands Cancer Institute (NKI) for biological testing.

The synthetic route of 1-(4-Bromophenyl)-N-methylmethanamine has been constantly updated, and we look forward to future research findings.

Reference:
Article; Milne, Kirsty; Sun, Jianhui; Zaal, Esther A.; Mowat, Jenna; Celie, Patrick H.N.; Fish, Alexander; Berkers, Celia R.; Forlani, Giuseppe; Loayza-Puch, Fabricio; Jamieson, Craig; Agami, Reuven; Bioorganic and Medicinal Chemistry Letters; vol. 29; 18; (2019); p. 2626 – 2631;,
Bromide – Wikipedia,
bromide – Wiktionary