Month: January 2021

Related Products of 699-03-6, 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 699-03-6 as follows.

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.

According to the analysis of related databases, 699-03-6, the application of this compound in the production field has become more and more popular.

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

Application of 3972-64-3, A common heterocyclic compound, 3972-64-3, name is 1-Bromo-3-(tert-butyl)benzene, molecular formula is C10H13Br, 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.

(9-1) Synthesis of (9-1)1-(t-butyl)-3-methylbenzene 1-Bromo-3-(t-butyl)benzene(20.26 g, 95.1 mmol) was dissolved in diethyl ether(200 mL), {1,1′-bis(diphenylphosphino)ferrocenyl}nickel dichloride(1.00 g, 1.46 mmol) was added. Solution of methylmagnesium bromide in diethyl ether(3.00 M, 35.00 mL) was dropped at -85¡ãC, and after elevating temperature naturally, reaction solution was stirred for 1 hour at -5¡ãC, and water(30 mL) was added. Solution was washed with hydrochloric acid and water, and organic layer was extracted with diethyl ether. Organic layer was dried over magnesium sulfate, then, solvent was distilled off to obtain the crude product. This was purified by silica-gel column chromatography to obtain the desired 1-(t-butyl)-3-methylbenzene(13.58 g, 91.6 mmol).

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; Japan Polypropylene Corporation; NAKANO, Masato; UCHINO, Hideshi; IWAMA, Naoshi; KASHIMOTO, Masami; KATO, Tomohiro; EP2360163; (2011); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

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

To a 500 ml three-neck bottle by adding 31.2g (0.1mol) I-18-b, 23.2g (0.11mol) 3,4,5-trifluorobromobenzene (reactant), 31.8g (0.3mol) sodium carbonate (reactant), 1g tetrakis(triphenylphosphine)palladium (catalyst), 80 ml toluene (solvent), 60 ml ethanol (solvent), 60 ml of deionized water (solvent), under the protection of nitrogen is heated to reflux, reflux the reaction for 6 hours, then cooled to room temperature, liquid, with 50 ml * 2 toluene extraction aqueous phase two, combined with the phase, and then using 100 ml * 2 saturated sodium chloride solution to wash the organic phase, dried with anhydrous sodium sulfate the organic phase, then filtering the desiccant, the concentrated to remove the solvent, after column chromatography using normal hexane-hexane recrystallization for 2 times, get 27.8g (0.07mol) I-14 of target product, yield: 70%.

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; Shijiazhuang Chengzhi Yonghua Display Materials Co., Ltd.,; HAN, YAOHUA; TIAN, QIUFENG; LIU, RENJIE; ZHANG, FANGMIAO; LI, HONGFENG; SHI, ZHENG; HUA, RUIMAO; (30 pag.)CN103787826; (2016); B;,
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. 10269-01-9, name is (3-Bromophenyl)methanamine, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 10269-01-9

General procedure: To a solution of2(5 mmol,1equiv) in DMF (10 mL) was added 3-bromobenzylamine (5 mmol, 1equiv) and K2CO3(5 mmol, 1equiv).Then the reaction mixture was stirred for 4 h at 90C. Then the mixture was quenched with water (50ml) and extracted with ethyl acetate (2¡Á50 mL).The combined organic layers werewashed with saturated NaCl solution anddried overanhydrous Na2SO4and concentrated under vacuumto give the corresponding target product3.

According to the analysis of related databases, 10269-01-9, the application of this compound in the production field has become more and more popular.

Reference:
Article; Yu, Yu; Ran, Dongzhi; Jiang, Junhao; Pan, Tao; Dan, Yanrong; Tang; Li, Wei; Zhang, Lin; Gan, LinLing; Gan, Zongjie; Bioorganic and Medicinal Chemistry Letters; vol. 29; 16; (2019); p. 2136 – 2140;,
Bromide – Wikipedia,
bromide – Wiktionary

6274-57-3, name is 1-(4-Bromophenyl)-N,N-dimethylmethanamine, belongs to bromides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. Recommanded Product: 6274-57-3

2-Methoxy-3-amino-5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyridine (200 mg, 0.80 mmol, 1 equivalent) was dissolved in toluene (8 mL) and ethanol (2 mL) and then 1-(4-bromophenyl)-N,N-dimethylmethylamine (205 mg, 0.96 mmol, 1.2 equiv-alents) was added followed by tetrakis(triphenylphosphine)palladium(0) (46.2 mg, 0.04 mmol, 0.05 equivalents). Sodium carbonate (585 mg, 5.52 mmol, 6.9 equivalents) and water (3.5 mL) were then added and the reaction mixture heated to reflux for 2 hours under argon. After cooling the solution was diluted with water (15 mL) and extracted with EtOAc (3×50 mL) and the organic layers collected and washed with brine. The organic layers were then dried over magnesium sulfate and concentrated. The residue was purified using an SCX column (eluted with 2 M ammonia in methanol) to give a grey solid (147 mg, 71.4%).

The synthetic route of 6274-57-3 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Fearon, Daren; Westwood, Isaac M.; van Montfort, Rob L.M.; Bayliss, Richard; Jones, Keith; Bavetsias, Vassilios; Bioorganic and Medicinal Chemistry; vol. 26; 11; (2018); p. 3021 – 3029;,
Bromide – Wikipedia,
bromide – Wiktionary

Adding a certain compound to certain chemical reactions, such as: 65896-11-9, name is 2-Bromo-6-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 65896-11-9, SDS of cas: 65896-11-9

2-Bromo-6-fluoroaniline (8.2 g, 43.2 mmol) was dissolved in pyridine (10 mL) and treated with pivaloyl chloride (7.0 mL, 57.2 mmol). The reaction was stirred at room temperature for 3 h. The reaction mixture was concentrated in vacuo and treated with ethyl acetate (50 mL). Mixture was washed 1 N hydrochloric acid (2¡Á), then brine. The organic layer was dried (magnesium sulfate), filtered, and concentrated in vacuo. The residue was triturated with hexanes to give a solid which was filtered, washed with hexanes, and dried in vacuo. The title compound was obtained as white solid in 76% yield. 1H NMR (300 MHz, CDCl3): delta 7.39-7.31 (m, 1H), 7.14-7.03 (m, 2H), 6.98 (bs, 1H), 1.34 (s, 9H). Mass spec.: 274.1 (MH)+, 276.1 (MNa)+.

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; Degnan, Andrew P.; Han, Xiaojun; Dubowchik, Gene M.; Macor, John E.; Mercer, Stephen E.; US2005/215576; (2005); A1;,
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. 586-61-8, name is 1-Bromo-4-isopropylbenzene, This compound has unique chemical properties. The synthetic route is as follows., Computed Properties of C9H11Br

A mixture of 30.0 g (0.20 mol) of 2-FORMYLPHENYLBORONIC acid, 43.8 g (0. 22 MOL) of 4-bromoisopropylbenzene, 91.0 g (0.60 mol) of caesium fluoride and 6.9 g (0.0060 mol) of tetrakis (triphenylphosphine) palladium (0) in 700 ml of 1,2-dimethoxyethane is refluxed under a nitrogen atmosphere for 3 hours. After cooling, 1.5 1 of diethyl ether and 1 1 of water are added to the reaction medium and the organic phase is separated out, dried over sodium sulfate and concen- trated. The oily residue obtained is purified by chromatography on a column of silica (eluent : 30/1 hexane/ethyl acetate) to give 25.3 g (56.4%) of a pale yellow oil corresponding to the title compound. NMR: (CDCI3) 8 (PPM) : 1.31 (6 H, d, J = 7 Hz); 2.99 (1 H, sept, J = 7 Hz); 7.26-7. 39 (4 H, m); 7.41-7. 53 (2 H, m); 7.54-7. 69 (1 H, m); 7.93-8. 13 (1 H, m); 10. 01 (1 H, s). I R : v (C =0) : 1694 CM~

According to the analysis of related databases, 586-61-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; MERCK PATENT GMBH; WO2004/37806; (2004); 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. 656-64-4, name is 3-Bromo-4-fluoroaniline, A new synthetic method of this compound is introduced below., Product Details of 656-64-4

4-(6-Chloro-4-(ethoxycarbonyl)chroman-7- yloxy)benzoic acid (Preparation 1) (0.214 g, 0.569 mmol) was dissolved in 1,2- dichloroethane (2 ml) and a drop of DMF was added. To the mixture was added oxalyl chloride (2M in dichloromethane) (0.313 ml, 0.626 mmol). Gas evolution was observed. The mixture was stirred for 2 hours at ambient temperature. A solution of 3-bromo-4- fluoroaniline (0.113 g, 0.597 mmol) and triethylamine (0.158 ml, 1.138 mmol) in dichloromethane (1 ml) was added to the acid chloride solution. The mixture was stirred for 0.5 hour and the crude mixture was purified on silica gel (EtOAc in hexanes gradient) to provide 0.2656 g of the title compound as a white solid (85%).

The synthetic route of 656-64-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ARRAY BIOPHARMA INC.; WO2009/158426; (2009); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Adding a certain compound to certain chemical reactions, such as: 445-02-3, name is 4-Bromo-2-(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 445-02-3, name: 4-Bromo-2-(trifluoromethyl)aniline

EXAMPLE 10 1-{3-Cyclopentyl-2-[4-(5-methyl-tetrazol-1-yl)-3-trifluoromethyl-phenyl]-propionyl}-3-methyl-urea A solution of 2-(trifluoromethyl)-4-bromoaniline (4.8 g, 20 mmol) in dry tetrahydrofuran (20 mL) was cooled to 0 C. and then treated with acetic anhydride (8.2 g, 80 mmol). The reaction mixture was stirred at 0 C. for 10 min and then allowed to warm to 25 C. The reaction mixture was stirred at 25 C. for 2 h, at which time, thin layer chromatography analysis of the reaction mixture indicated the absence of starting material. The reaction mixture was then concentrated in vacuo. The crude residue precipitated from diethyl ether (50 mL) and hexanes (50 mL). The solid was collected by filtrated and washed with hexanes to afford N-(4-bromo-2-trifluoromethyl-phenyl)-acetamide (5.07 g, 90%) as an amorphous white solid: EI-HRMS m/e calcd for C9H7BrF3NO (M+) 281.8352, found 281.8348.

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, 4-Bromo-2-(trifluoromethyl)aniline, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Sidduri, Achyutharao; US2002/35266; (2002); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Application of 111721-75-6, A common heterocyclic compound, 111721-75-6, name is 2-Bromo-3-fluoroaniline, molecular formula is C6H5BrFN, 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.

To a stirred solution of 2-bromo-3-fluoroaniline (5.00 g, 26.3 mmol) in dry THF (50 mL) at 0 C under nitrogen atmosphere was added pyridine (3.18 mL). Then 3- chloropropanoyl chloride (3.02 mL g, 31.6 mmol) was added in dropwise carefully. Then the reaction mixture was warmed to room temperature and stirred for 16 hours. After that the reaction mixture was concentrated under reduced pressure. The residue obtained was diluted with water (100 mL) and extracted with ethyl acetate (3 x 75 mL). The combined extract was washed with water, brine, dried over Na2S04 and concentrated in vacuo to get compound Xa (crude), which was used for the next step without any further purification. Yield: 6.40 g; -NuMuIota (400 MHz, DMSO-d6): 9.77 (s, 1H), 7.48 – 7.39 (m, 2H), 7.24 – 7.19 (m, 1H), 3.88 (t, = 6.4 Hz, 2H), 2.91 (t, = 6.4 Hz, 2H)

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; BUGWORKS RESEARCH INDIA PVT LTD; PEER MOHAMED, Shahul Hameed; BHARATHAM, Nagakumar; KATAGIHALLIMATH, Nainesh; SHARMA, Sreevalli; NANDISHAIAH, Radha; RAMACHANDRAN, Vasanthi; VENKATARAMAN, Balasubramanian; (221 pag.)WO2018/225097; (2018); A1;,
Bromide – Wikipedia,
bromide – Wiktionary