Month: March 2021

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. 68322-84-9, name is 2-Bromo-1-fluoro-4-(trifluoromethyl)benzene, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 2-Bromo-1-fluoro-4-(trifluoromethyl)benzene

Example 2 [0028] [0029] A 400 mL shaker tube was loaded with 50 g of 3-bromo-4-fluorobenzotrifluoride and 10 g of SbF5. The shaker tube was evacuated, charged with 20 g of TFE, and agitated for 12 h at 25 C. The crude product was unloaded from the shaker tube and washed with water. The organic layer was separated, dried over MgSO4 and filtered to give 37 g of crude product, containing benzotrifluoride and compounds 4 and 5 in a ratio of 10:60:30, respectively, as determined by NMR and GC/MS. The reaction mixture was distilled at atmospheric pressure, using a spinning-band distillation column to give 15.3 g of a fraction (b.p. 142-144 C. at 760 mm Hg) and 13.5 g of residue. According to NMR analysis, the distilled fraction contained compounds 4 and 5 in a ratio of 85:15. The residue was found to be a mixture of 4 and 5 in a ratio of 30:70. [0030] Compound 4. 19F NMR (CDCI3): -80.38 (3F,t), -101.28 (1F, m), -111.56 (2F,m), -126.61(2F, s) ppm. H1 NMR (CDCl3): 7.32 (1H,m), 7.70 (1H,m), 7.92 (1H,m) ppm. [0031] Compound 5. 19F NMR (CDCl3): -79.33 (6F, m)), -102.46 (1F,m), -120.33 (4F, A:B quartet), -181.75, 1F, m) ppm. H1 NMR (CDCl3): 7.32 (1H,m), 7.70 (1H,m), 7.92 (1H,m) ppm.

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 68322-84-9.

Reference:
Patent; E I DU PONT DE NEMOURS AND COMPANY; Petrov, Viacheslav A.; US2014/200372; (2014); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

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 201138-91-2 as follows. Recommanded Product: 4,6-Dibromodibenzo[b,d]furan

6.48 g (20 ml) of 4,6-dibromodibenzo[b,d]furan was dissolved in 100 ml of THF, and 8 ml (2.5 M in hexane) of normal butyllithium was added thereto at about -78 C. After one hour, 1.36 ml (10 mmol) of dichlorophenylphosphine was slowly added dropwisely and stirred for about 3 hours. The temperature was increased to room temperature, water was added, and then, the solution was washed with ethyl acetate (30 ml) three times. The washed ethyl acetate layer was dried with magnesium sulfate (MgSO4) and dried at a reduced pressured to produce a crude product. The crude product thus obtained was separated by silica gel column chromatography to obtain 4.19 g of Intermediate I-23(yield 70%). The product thus obtained was identified by LC-MS (C30H17Br2O2P: M+1 598.0).

According to the analysis of related databases, 201138-91-2, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Samsung Display Co., Ltd.; PARK, Junha; SIM, Mun-ki; LEE, Hyoyoung; JEONG, Eunjae; KIM, Youngkook; HWANG, Seokhwan; (71 pag.)US2018/166639; (2018); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

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. 7745-91-7, name is 3-Bromo-4-methylaniline belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Application In Synthesis of 3-Bromo-4-methylaniline

General procedure: 1-Aryl-4-nitro-1H-imidazoles were prepared following the general procedure we have developed in our laboratory [23] with some slight modifications. Equimolar amount of aniline derivative was treated with 1,4-dinitro-1H-imidazole in aqueous methanol at ambient temperature in the dark for several hours until complete disappearance of 1,4-dinitro-1H-imidazole monitored by TLC. In some cases, the mixture was heated under reflux to complete the reaction. On cooling, the desired crude 1-aryl-4-nitro-1H-imidazoles separated from the mixture by precipitation. After filtration and recrystallization the pure product was obtained. Yields, solvents used for recrystallization and specific data are given below in the respective sections. Further details are available on request.

The synthetic route of 7745-91-7 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Trunz, Bernadette Bourdin; Jdrysiak, Rafa?; Tweats, David; Brun, Reto; Kaiser, Marcel; Suwi?ski, Jerzy; Torreele, Els; European Journal of Medicinal Chemistry; vol. 46; 5; (2011); p. 1524 – 1535;,
Bromide – Wikipedia,
bromide – Wiktionary

Electric Literature of 583-75-5,Some common heterocyclic compound, 583-75-5, name is 4-Bromo-2-methylaniline, molecular formula is C7H8BrN, 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.

Potassium acetate (317 mg, 3.22 mmol), 4,4,4′,4′,5,5,5′,5′-octamethyl-2,2′-bi(1,3,2-dioxaborolane) (300 mg, 1.18 mmol) and 4-bromo-2-methyl-aniline (200 mg, 1.08 mmol) were dissolved in dimethylsulfoxide (3 mL). The reaction mixture was degassed using argon. 1,1′-Bis-diphenylphosphine ferrocene palladium(II) dichloride (24 mg, 0.03 mmol) was added and the reaction mixture was heated at 80 C for 5 h. The reaction mixture was cooled to room temperature and diluted with ethyl acetate (20 mL). The organic layer was washed with saturated sodium bicarbonate (20 mL) and brine (20 mL). The organic layer was dried with sodium sulfate, filtered and purified by flash silica column chromatography (heptane:ethyl acetate, 0-40%) to obtain a crude mixture of starting material and product. The mixture was purified using reversed phase column chromatography to obtain the title compound as a clear oil (50 mg, 21%). ESI-MS m/z: 234 (M+H)+.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 4-Bromo-2-methylaniline, its application will become more common.

Reference:
Patent; Emergent Product Development Gaithersburg Inc.; Roussel, Patrick; Heim, Jutta; Schneider, Peter; Bartels, Christian; Liu, Yaoquan; Dale, Glenn; Milligan, Daniel; (107 pag.)EP3034078; (2016); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Synthetic Route of 7051-34-5, A common heterocyclic compound, 7051-34-5, name is (Bromomethyl)cyclopropane, molecular formula is C4H7Br, 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.

A 15 g quantity of methyl 3-hydroxy-4-methoxybenzoate obtained in Reference Example 1 was dissolved in 150 ml of dimethylformamide, and 34 g of potassium carbonate and 22.2 g of (bromomethyl) cyclopropane were added. The mixture was heated at 9O0C overnight. Ice water was added to the reaction mixture, and the precipitated crystals were collected by filtration and washed with an excess of water. The obtained crystals were dried under reduced pressure at room temperature to give 18.3 g of white crystalline methyl 3-cyclopropylmethoxy-4-methoxybenzoate. 1H-NMR (CDCl3) delta: 7.67 (IH, dd, J = 8.4, 1.8 Hz), 7.52 (IH, d, J = 2.1 Hz), 6.89 (IH, d, J = 8.4 Hz), 3.94-3.86 (8H, m) , 1.43-1.29 (IH, m), 0.70-0.58 (2H, m) , 0.45-0.30 (2H, m)

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; OTSUKA PHARMACEUTICAL CO., LTD.; WO2007/58338; (2007); A2;,
Bromide – Wikipedia,
bromide – Wiktionary

Synthetic Route of 4101-68-2, The chemical industry reduces the impact on the environment during synthesis 4101-68-2, name is 1,10-Dibromodecan, I believe this compound will play a more active role in future production and life.

General procedure: The bromide or iodide salts of 1,n-bis(isoquinolinium)alkane dications (n = 2, 4, 5, 6, 8, 9, 10 and 12) and alpha,alpha’-bis(isoquinolinium)-p-xylene dibromide were prepared using modifications of a method outlined by Kuca et al.. A mixture of the appropriate 1,n-bis(isoquinolinium)alkane dibromide or diiodide (1.0 mmol) or alpha,alpha’-dibromo-p-xylene (1.0 mmol) and isoquinoline (9.0 mmol) in DMF was heated at 70 C for 1-4 days. The addition of diethyl ether to the cooled solution resulted in a light brown precipitate, which was filtered and washed with diethyl ether.

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, 1,10-Dibromodecan, other downstream synthetic routes, hurry up and to see.

Reference:
Conference Paper; Kwok, Julian C.; Macartney, Donal H.; Supramolecular Chemistry; vol. 26; 3-4; (2014); p. 182 – 191;,
Bromide – Wikipedia,
bromide – Wiktionary

Application of 1000994-95-5, The chemical industry reduces the impact on the environment during synthesis 1000994-95-5, name is 1-Bromo-4-(1,1-difluoroethyl)benzene, I believe this compound will play a more active role in future production and life.

In a 40 ml vial, bromo derivative (250 mg, 1.13 mmol, 1.0 eq.), bispinacolotodiboron (288.6 mg, 1.13 mmol, 1.0 eq.), Pd(dppf)CI2 (92.7 mg, 0.114 mmol, 0.1 eq.) and potassium acetate (354.5 mg, 3.41 mmol, 3.0 eq.) were mixed in dioxane (10 ml) and heated to 80 C for 8 hours. LCMS indicated that the product was formed in major amount. . The crude reaction was purified in the presence of silica (10-15 gm) and purified using hexanes: ethyl acetate (0-100%) to yield desired boron ester. The product was characterized by reverse phase HPLC using method 4. (ES, m/z) [M + H+] 269.0. Retention time = 1.60 mins.

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-4-(1,1-difluoroethyl)benzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; IRM LLC; NOVARTIS AG; CHATTERJEE, Arnab Kumar; NAGLE, Advait Suresh; PARASELLI, Prasuna; LEONG, Seh Yong; ROLAND, Jason Thomas; MISHRA, Pranab Kumar; YEUNG, Bryan KS; ZOU, Bin; WO2014/78813; (2014); 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. 556-96-7, name is 1-Bromo-3,5-dimethylbenzene, This compound has unique chemical properties. The synthetic route is as follows., Computed Properties of C8H9Br

2-bromo-3,5-dimethylbenzene 15a (1.06 g, 5.70 mmol), bis(pinacolato)diboron (2.0 g, 8.60 mmol),1,1 ‘-bis (diphenylphosphino) ferrocene] dichloropalladium (210 mg, 0.20 mmol) and potassium acetate (1.40 g, 14.30 mmol) was dissolved in 20 mL of ethylene glycol dimethyl ether and heated to reflux for 3 hours. Filtered, and the filtrate was concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography using eluent system B to give the title product, 2-(3,5-dimethylphenyl)-4,4,5,5-tetramethyl-1,3,2-dioxaborolane 15b (538 mg, yellow oil), yield: 42.1%.

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 556-96-7.

Reference:
Patent; SHANGHAI HENGRUI PHARM CO LTD; JIANGSU HENGRUI MEDICINE CO LTD; Lyu, HEJUN; DONG, QING; FEI, HONGBO; JIANG, HONGJIAN; SONG, PENG; (114 pag.)CN103030646; (2016); B;,
Bromide – Wikipedia,
bromide – Wiktionary

Some common heterocyclic compound, 18648-66-3, name is 2-(4-Bromophenyl)-1,1-diphenylethylene, molecular formula is C20H15Br, 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. Formula: C20H15Br

(1) Synthesis of 2-(2-biphenylyl)-9,10-bis(4-(2,2-diphenylvinyl)phenyl)-9,10-dihydroxy-9,10-dihydro anthracene; [Compound (B1-0)]; Under an atmospheric argon gas flow, 4-(2,2-diphenylvinyl)-1-bromobenzene in an amount of 9.8 g (29 mmol, 3 eq) was dissolved into a mixed solvent of anhydrous toluene in an amount of 45 milliliter and anhydrous THF in an amount of 45 milliliter, followed by cooling down to the temperature of – 20 C by means of dry ice / methanol bath. Adding hexane solution of n-butyllithium in an amount of 19 milliliter (1.59 mol/litter, 30 mmol; 1.04 eq), the resultant solution was stirred at the temperature of -20 C for 1 hour. Into the resultant solution, 2-(2-biphenylyl)-9,10-anthraquinone [Compound (A)] in an amount of 3.5 g (9.7 mmol) was added and after stirring at the room temperature for 2 hours, it was stood alone for a night. The resultant reaction mixture was deactivated with the use of saturated ammonium chloride aqueous solution in an amount of 50 milliliter, and the resultant solid was separated. The solid was washed use of the mixed solvent of hexane : dichloromethane = 1:1 (capacity ratio) and as a result, 5.0 g of white solid compound was obtained (yield: 59 %). The white solid was identified as the Compound (B1-0) in accordance with 1H-NMR. The measurement results of 1 H-NMR are shown as the following: 1H-NMR (CDCl3, TMS) delta 2.17 (1H, s), 2.66 (1H, s), 6.21 (2H, d, J=8Hz), 6.51 (2H, d, J=8Hz), 6.55 (4H, s), 6.80 (2H, d, J=4Hz), 7.0-7.4 (3H, m), 7.6-7.7 (3H, m)

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 18648-66-3, its application will become more common.

Reference:
Patent; IDEMITSU KOSAN CO., LTD.; EP1695952; (2006); 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. 1073-39-8, name is 3-Bromobicyclo[4.2.0]octa-1,3,5-triene, This compound has unique chemical properties. The synthetic route is as follows., COA of Formula: C8H7Br

A) Synthesis of N,N?-diphenyl-N,N?-dibenzocyclobutane-1,4-phenylenediamine (3) (0157) To a 500 ml, 3-neck round bottom flask equipped with a mechanical stirrer, nitrogen inlet, and reflux condenser (with nitrogen outlet), palladium (II) acetate (173 mg, 0.80 mmol) and tri(o-tolyl)phosphine (486 mg, 1.60 mmol) are added to 50 ml toluene. The mixture is stirred at room temperature under nitrogen until the palladium catalyst dissolves and the solution turns yellow. N,N?-diphenyl-1,4-phenylenediamine (10.0 g, 38.4 mmol), bromobenzocyclobutane (15.5 g, 76.8 mmol) and 200 ml toluene are added, followed by sodium t-butoxide (7.37 g, 76.8 mmol). Upon addition of the sodium t-butoxide the reaction turns black. The reaction is heated to reflux under nitrogen for 22 hours. The reaction is quenched by addition of 30 ml of 1 M aqueous HCl. The toluene solution is passed through basic alumina and the crude product is purified by recrystallization from a toluene/hexanes/methanol mixture. (0158) Yield=9.43 g (53 percent). 1H NMR (THF-d8) delta: 7.15 (t, 4H, Ar), 6.80-7.01 (m, 16H, Ar) 3.09 (s, 8H, -CH2CH2-) 13C-NMR (THF-d8) delta: 149.72, 148.26, 147.34, 144.18, 141.50, 129.92, 125.82, 125.76, 124.35, 123.61, 122.45, 121.06, 29.78.

According to the analysis of related databases, 1073-39-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; SUMITOMO CHEMICAL COMPANY, LIMITED; Gaynor, Scott; Inbasekaran, Michael; O’Brien, James J.; Welsh, Dean M.; (20 pag.)US9399702; (2016); B2;,
Bromide – Wikipedia,
bromide – Wiktionary