Month: June 2021

Adding a certain compound to certain chemical reactions, such as: 1003-99-2, name is 2-Bromo-5-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 1003-99-2, Safety of 2-Bromo-5-fluoroaniline

To a solution of 2-bromo-5-fluoroaniline (1.0 eq.) in tetrahydrofuran (0.2 M) at 0° C. under N2 atmosphere was added dropwise 1M NaHMDS (2.5 eq.). The reaction was stirred for 15 minutes at 0° C., and a solution of di-tert-butyl dicarbonate in tetrahydrofuran was added. The reaction was warmed to room temperature overnight. The solvent was evaporated, and the resulting residue was quenched with 0.1N HCl aqueous solution. The aqueous suspension was extracted twice with ethyl acetate. The combined organic layers were washed with brine, dried over anhydrous MgSO4, and concentrated en vacuo. The crude material was purified by flash chromatography on a COMBIFLASH® system (ISCO) using 0-5percent ethyl acetate in hexane to give the product as light yellow oil.

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, 2-Bromo-5-fluoroaniline, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; GlaxoSmithKline Biologicals SA; Skibinski, David; Jain, Siddhartha; Singh, Manmohan; O’Hagan, Derek; (124 pag.)US9408907; (2016); B2;,
Bromide – Wikipedia,
bromide – Wiktionary

Related Products of 61326-44-1, The chemical industry reduces the impact on the environment during synthesis 61326-44-1, name is 1,1,2,2-Tetrakis(4-bromophenyl)ethene, I believe this compound will play a more active role in future production and life.

Using the polar solvent “one-pot synthesis”, the 1, 1, 2, 2-tetra (4-bromophenyl) ethylene, 1H-1, 2, 4-triazole, potassium carbonate, and copper oxide in the preparation of the heating condition; wherein the 1, 1, 2, 2-tetra (4-bromophenyl) ethylene: 1H-1, 2, 4-triazole: potassium carbonate: copper oxide in a molar ratio of 2:10-15 : 30:1; the reaction temperature 80-200°C, reaction time 12-120 hours. The present invention is preferably 1, 1, 2, 2-tetra (4-bromophenyl) ethylene: 1H-1, 2, 4-triazole: potassium carbonate: copper oxide in a molar ratio of 2:10-15 : 30:1; the reaction temperature is 100 °C, the reaction time is 48 hours. In the polar solvent, the “one-pot synthesis”, the 1, 1, 2, 2-tetra (4-bromophenyl) ethylene, 1H-1, 2, 4-triazole, potassium carbonate, and copper oxide under the heating condition preparing 1, 1, 2, 2-tetra [4 – (1H-1, 2, 4-triazole-1-yl) phenyl] ethylene (L). Yield 60percent

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, 1,1,2,2-Tetrakis(4-bromophenyl)ethene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Tianjin Normal University; Wang, yin; (12 pag.)CN105418655; (2016); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Application of 2635-13-4, 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. 2635-13-4 name is 5-Bromobenzo[d][1,3]dioxole, 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.

A heavy-walled tube was charged with 5.01 grams (3 ml, 24.896 mmol) ofcommercially available 5-bromo-1,3-benzodioxole followed by dry DMF (5ml) followed by copper iodide (0.474 grams, 2.490 mmol, 0.10 equivalents), PdCl2(PPh3)2 (0.349 grams, 0.4979 mmol, 0.02 equivalents), and triethylamine (35 ml) and then subjected tooxygen removal using a freeze-pump-thaw method. Finally TMS-acetylene (3.68 grams, 5.3 ml,37.34 mmol) was then added and the tube was quickly sealed and heated in an oil bath at 90 Cfor 24 hours. At this time the reaction was cooled and worked up by concentration in vacuo andsubmitted to flash chromatography using straight hexanes to afford compound weighing 3.4 g.Yield is 62 %.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 5-Bromobenzo[d][1,3]dioxole, and friends who are interested can also refer to it.

Reference:
Article; Abrams, Jason N.; Zhao, Qi; Ghiviriga, Ion; Minaruzzaman; Tetrahedron; vol. 68; 2; (2012); p. 423 – 428;,
Bromide – Wikipedia,
bromide – Wiktionary

These common heterocyclic compound, 22385-77-9, name is 1-Bromo-3,5-di-tert-butylbenzene, 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. Safety of 1-Bromo-3,5-di-tert-butylbenzene

Production Example 2 of Optically Active AminoalcoholA 200 mL round-bottom four-neck flask equipped with a Dimroth condenser with a nitrogen introducing tube attached thereto, a thermometer, a magnetic rotator and a dropping funnel was heated under reduced pressure, nitrogen was then introduced into the flask, pressure in the flask was returned to normal pressure, and the flask was cooled to room temperature. After 1.27 g of magnesium and a minor amount of iodine were added to the flask, a small amount of a solution obtained by mixing 15.00 g of 3,5-di-tert-butylbromobenzene and 75.0 mL of dehydrated tetrahydrofuran was added dropwise. The flask was heated, and it was confirmed that the Grignard reaction was initiated. Thereafter, the remaining solution was added dropwise to the flask over 30 minutes. The resulting mixture was refluxed for 1.5 hours. After the resulting reaction mixture was cooled to -10° C., 1.11 g of L-valine methyl ester hydrochloride was added. After the temperature of the resulting mixture was raised to room temperature, the mixture was further refluxed for 4 hours. The resulting reaction mixture was cooled to 0 to 5° C. To the reaction solution were added dropwise 45.0 mL of an aqueous saturated ammonium chloride solution, and further 15.0 mL of water. The resulting mixture was stirred at 20° C. for 30 minutes. The resulting mixture was extracted with 45.0 mL of diethyl ether three times. The resulting organic layers were mixed, and dried with anhydrous sodium sulfate. After sodium sulfate was removed by filtration, the resulting filtrate was concentrated. The resulting residue was purified by silica gel column chromatography (ethyl acetate/hexane=2/9840/60) to obtain 1.02 g of a colorless crystal of (S)-2-amino-1,1-di(3,5-di-tert-butylphenyl)-3-methyl-1-butanol.1H-NMR (300 MHz, CDCl3, TMS standard)delta (ppm): 7.54 (2H, d), 7.43 (2H, d), 7.28 to 7.24 (2H, m), 4.23 (1H, brs), 3.80 (1H, d), 1.77 (1H, m), 1.35 (18H, s), 1.33 (18H, s), 1.32 (2H, s), 0.96 (3H, d), 0.87 (3H, d)13C-NMR (75 MHz, CDCl3, TMS standard)delta (ppm): 150.86, 150.43, 147.46, 144.67, 121.01, 120.80, 120.76, 120.38, 81.24, 62.12, 35.67, 35.61, 32.33, 32.27, 28.60, 23.88, 17.09

The synthetic route of 1-Bromo-3,5-di-tert-butylbenzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Masumoto, Katsuhisa; Yoshikawa, Kouji; US2011/166372; (2011); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Related Products of 22385-77-9,Some common heterocyclic compound, 22385-77-9, name is 1-Bromo-3,5-di-tert-butylbenzene, molecular formula is C14H21Br, 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.

The bromide (2.0 g, 7.4 mmol), tri-nbutyi-1-ethoxyvinyl tin (3.2 g, 8.9 mmol), and PdCl2(Ph3P)2 ( 522 mg, 0.74 mmol) were dissolved in toluene 3.7 mL and the solution stirred at 95 0C for 3 hours. The volatiles were removed in vac. and the residue dissolved in 1,4-dioxane (33 mL). Aqueous HCl (2 N, 1 1 mL) was added and the solution stirred rapidly at RT for 1 hour. The mixture was diluted with water (350 mL), followed by aqueous/EtOAc work-up and silica gel chromatography (diethyl ether: hexanes (1 :9)) to give the titled compound.

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-3,5-di-tert-butylbenzene, its application will become more common.

Reference:
Patent; MERCK & CO., INC.; WO2007/64553; (2007); A2;,
Bromide – Wikipedia,
bromide – Wiktionary

Application of 55289-36-6, 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. 55289-36-6, name is 3-Bromo-2-methylaniline belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To a flask containing aqueous sulfuric acid (14%, 260 mL), 3-bromo-2-methylaniline (5.00 mL, 40.6 mmol) was added. The mixture was brought to reflux, and a solution of sodium nitrite (3.08 g, 44.6 mmol) in water (minimum amount required to dissolve) was added dropwise over the course of 1 hour. The mixture was refluxed an additional 30 minutes, cooled to room temperature, and extracted three times with chloroform. The combined chloroform layeres were extracted three times with aqueous sodium hydroxide (1 M). The aqueous layers were acidified with concentrated hydrochloric acid and extracted three times with chloroform. These three chloroform extracts were combined, dried over magnesium sulfate, filtered, and concentrated to give 3-bromo-2-methylphenol (10-1, 5.63 g) as a brown 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-2-methylaniline, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Aviara Pharmaceuticals, Inc.; Biediger, Ronald J.; Benish, Michele A.; Hardy, Lindsay Bonner; Boyd, Vincent A.; Market, Robert V.; Thrash, Thomas P.; Young, Brandon M.; (83 pag.)US2018/312523; (2018); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Reference of 337915-79-4, A common heterocyclic compound, 337915-79-4, name is 5-Bromo-N1-methylbenzene-1,2-diamine, molecular formula is C7H9BrN2, 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.

[000821j To a stirred solution of compound 1 (2 g, 1 eq) in THF (40 mL), CDI (2.42 g, 1.5 eq) was added and heated to reflux for 18 h. The progress of the reaction was monitored by TLC. After completion of the reaction, the reaction mixture was evaporated under reduced pressure. The residue was diluted with ethyl acetate (100 mL) and washed with water. Organic layer was dried over anhydrous sodium sulfate and evaporated under reduced pressure to afford the crude compound 2. LCMS (mlz): 226.90 (M + 1).

The synthetic route of 337915-79-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BIOMARIN PHARMACEUTICAL INC.; BHAGWAT, Shripad; WANG, Bing; LUEDTKE, Gregory R.; SPYVEE, Mark; (490 pag.)WO2016/57834; (2016); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Reference of 5003-71-4, 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. 5003-71-4, name is 3-Bromopropan-1-amine hydrobromide belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

A solution of 3-bromopropylamine hydrobromide (1.0 g, 4.6 mmol) in a 2:1 dioxane/H2O (45 mL) was cooled to 0 C. and treated with K2CO3 (6.22 g, 45 mmol) and di-tert-butyl dicarbonate (1.5 g, 6.9 mmol). The reaction was stirred for 15 h while warming to room temperature. The dioxane was removed in vacuo and the remaining aqueous mixture was acidified with 5 N HCl and extracted with ethyl acetate (5*25 mL). The combined organic layers were dried with MgSO4 and yielded 3-bromo-N-(tert-butoxycarbonyl)propylamine as a colorless oil (0.93 g, 93%). 1H-NMR (CDCl3/TMS, ppm): 1.41 (s 9H, CH3), 2.02 (quintet, J=6.4 Hz, 2H, CH2), 3.23 (m, 2H, NCH2), 3.41 (t, J=6.6 Hz, CH2Br), 4.8 (broad, 1H, NH); 13C-NMR (CDCl3, ppm): 28.3 (CH3), 30.7, 32.6, 38.9 (CH2), 79.3 (quaternary C), 155.9 (CO); MS (CI, m/z): 239, 241 (M+H+ Calc. for C8H16BrNO2 237.03644).

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-Bromopropan-1-amine hydrobromide, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Research Development Foundation; US6703384; (2004); B2;,
Bromide – Wikipedia,
bromide – Wiktionary

Related Products of 4117-09-3,Some common heterocyclic compound, 4117-09-3, name is 7-Bromo-1-heptene, molecular formula is C7H13Br, 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 alkyl bromide (1.0 equiv) was added to a solution of mercaptoaceticacid (1.0 equiv) in methanol (10.0 mL) and the resultingsolution stirred. Then a solution of NaOH (2.0 equiv) in methanol(5.0 mL)was added slowly, and the final mixturewas stirred at roomtemperature or heated to reflux until absence of the alkyl bromide(checked by TLC). The reaction mixture was concentrated in vacuo,diluted with H2O, and neutralized with 1 N HCl. Then the obtainedreaction mixture was extracted with EtOAc. The combined organicfractions were washed with brine, dried with Na2SO4, and concentratedin vacuo. Purification of the crude residue by column chromatography(petroleum ether/EtOAc) afforded the title compound.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 7-Bromo-1-heptene, its application will become more common.

Reference:
Article; Chen, Ying; Wu, Bolin; Hao, Yameng; Liu, Yunqi; Zhang, Zhili; Tian, Chao; Ning, Xianling; Guo, Ying; Liu, Junyi; Wang, Xiaowei; European Journal of Medicinal Chemistry; vol. 171; (2019); p. 420 – 433;,
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. 7073-94-1, name is 1-Bromo-2-isopropylbenzene, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 1-Bromo-2-isopropylbenzene

Step I: To a solution of 2-bromoisopropyl benzene (2.0 g, 10.0 mmole) in dry THF (20 mL), nBuLi (1.6 M in hexane), (6.9 mL, 11.05 mmole) was added at -78 C. and the mixture was stirred at same temperature for one hour. DMF (0.9 g, 12.0 mmole) was added and the mixture was stirred at -78 C. for half an hour then allowed to stir at 0 C. for 15 min. The reaction mixture was diluted with saturated aqueous ammonium chloride (10 mL) and extracted with EtOAc (3*30 mL). The organic layers were combined and washed with brine, dried over sodium sulfate, and concentrated to yield 2-isopropyl benzaldehyde (1.4 g).

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 7073-94-1.

Reference:
Patent; NOVARTIS AG; US2011/171159; (2011); A1;,
Bromide – Wikipedia,
bromide – Wiktionary