Month: March 2021

Related Products of 51437-00-4, 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. 51437-00-4, name is 4-Bromo-1-fluoro-2-methylbenzene belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

4-Bromo-2-bromomethyI-l-fluoro-benzene (TJA01131) C7H5Br2F MW 267.92. 5-bromo-2-fluorotoluene (5.00 g, 26.5 mmol), N-bromosuccinimide (5.18 g, 29.1 mmol), benzyl peroxide (0.205 gs 0.850 mmol) and carbon tetrachloride (50 mL) were loaded to a -r.b. flask and set to reflux (79 0C) for 2 h. Once cooled the succinimide was filtered off and carbon tetrachloride removed via a dry ice-acetone cooled rotary evaporator. The residues were dissolved in dichloromethane (100 mL) and washed with distilled H2O (50 mL x 3) and brine (50 mL). Dried over MgSO4 and solvent removed in vacuo to yield the title compound as a colourless liquid yellow (6.80 g, 96 %), R/. 0.55 (dichloromethane/hexane 10:90), c.f. 0.79 (5-bromo-2-fluorotoluene); HPLC (70 % CH3CN in H2O) tr=4.786 (71.55 %).

The synthetic route of 4-Bromo-1-fluoro-2-methylbenzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; STERIX LIMITED; WO2007/68905; (2007); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Adding a certain compound to certain chemical reactions, such as: 955959-84-9, name is 4-(4-Bromophenyl)dibenzo[b,d]furan, 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 955959-84-9, HPLC of Formula: C18H11BrO

Intermediate M-1 in a round bottom flask 10.0g (30.9mmol) and M-32 15.5g (30.9mmol),Sodi um-t- butoxide placed 4.46g (46.35mmol) was dissolved was added to 155ml of toluene. Here Pd2 (dba) 3 0.28g (0.31mmol) and tri-tert-butylphosphine was placed to 0.18g (0.93mmol) in turn and the mixture was stirred under reflux for 12 hours under a nitrogen atmosphere. After the reaction extracted with distilled water and toluene and the organic layer was dried with magnesium sulfate, filtered and the filtrate was concentrated under reduced pressure. The product n- hexane / dichloromethane (8: 2 by volume) to yield the silica gel column chromatography to give compound 9 as 20.71g (90percent yield).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 4-(4-Bromophenyl)dibenzo[b,d]furan, and friends who are interested can also refer to it.

Reference:
Patent; SAMSUNG SDI CO., LTD.; JANG, YU NA; HONG, JIN SEOK; KIM, YOUNG KWON; YU, EUN SUN; KIM, CHANG WOO; KIM, HUN; MIN, SOO HYUN; CHO, PYEONG SEOK; (38 pag.)KR2016/12846; (2016); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Application of 6138-90-5,Some common heterocyclic compound, 6138-90-5, name is Geranyl bromide, molecular formula is C10H17Br, 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.

Example 26(4E)-2-(4-Methoxy-benzenesulfonyl)-5,9-dimethyl-2-[4-(2-morpholin-4-yl-ethoxy) – benzyl]-deca-4,8-dienoic acid hydroxyamide To a stirred solution of (4-methoxy-benzenesulfonyl)-acetic acid ethyl ester (5.16 g, 20 mmol), geranyl bromide (4.2g, 20 mmol) and 18-Crown-6 (500 mg) in acetone (250 ml) was added K2CO3 (10 gms, excess) and the mixture refluxed foe 24 hours. At the end, the reaction mixture was filtered and the acetone layer was concentrated. The residue obtained was extracted with chloroform, washed well with water, dried over anhydrous MgSO4, filtered and concentrated. The product obtained was purified by silica-gel column chromatography, eluting with 30% ethy acetate: hexane. The product 2-(4-methoxy-benzenesulfonyl)-5,9-dimethyl-deca-4,8-dienoic acid ethyl ester was isolated as a colourless oil. Yield: 7.0 g, 89%.

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

Reference:
Patent; Wyeth Holdings Corporation; EP970046; (2003); B1;,
Bromide – Wikipedia,
bromide – Wiktionary

Related Products of 3344-70-5,Some common heterocyclic compound, 3344-70-5, name is 1,12-Dibromododecane, molecular formula is C12H24Br2, 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.

1.0 g of compound 3,2.63 g of 1,12-dibromododecane,0.43 g of potassium hydroxide and 0.16 g of tetrabutylammonium bromide,Was added to a mixture of 10 ml of dichloromethane and 6.5 ml of water,The mixture was stirred at room temperature under nitrogen for 24 hours,With 30 millilitersWashed twice with water, washed once with 15 ml of saturated brine, the organic layer was separated, dried over anhydrous sodium sulfate,The solvent was removed on a rotary evaporator and purified by chromatography on a 200-300 mesh silica gel column (eluent ethyl acetate / petroleum ether volume ratio1: 30-1: 10) to give 1.19 g of compound 4 as a pale yellow liquid in 90percent yield.

The synthetic route of 3344-70-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Guilin University of Technology; Kong, Xiangfei; Dai, Shengping; Yang, Willow; Deng, Sea; Wang, Guixia; (8 pag.)CN106117224; (2016); A;,
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. 33884-43-4, name is 2-(2-Bromoethyl)-1,3-dioxane, This compound has unique chemical properties. The synthetic route is as follows., SDS of cas: 33884-43-4

Synthesis Example 9 Synthesis of 3-(1,3-Dioxan-2-yl)-1-(5-norbornen-2-yl)-1-propanol (Monomer 9) A Grignard reagent was customarily prepared from 36.2 g of 2-(2-bromoethyl)-1,3-dioxane in 200 ml of dry tetrahydrofuran. Then 19.5 g of 5-norbornene-2-carbaldehyde was added dropwise over 30 minutes to the Grignard reagent at 20 C. Stirring was continued for 30 minutes whereupon the reaction solution was added to a saturated aqueous solution of ammonium chloride to stop reaction. After diethyl ether extraction, the organic layer was successively washed with water, saturated sodium bicarbonate water and saturated sodium chloride water, dried over anhydrous sodium sulfate, and concentrated in vacuum. It was further purified by vacuum distillation, obtaining 36.2 g of 3-(1,3-dioxan-2-yl)-1-(5-norbornen-2-yl)-1-propanol (boiling point 125 C./27 Pa, yield 95%). IR (thin film): nu=3440 (br.), 3056, 2962, 2860, 2731, 2657, 1570, 1448, 1404, 1377, 1336, 1284, 1240, 1146, 1093, 1047, 997, 926, 721 cm-1; 1H-NMR (300 MHz in CDCl3): delta=0.45-2.35 (12H, m), 2.55-3.50 (3H, m), 3.65-3.80 (2H, m), 4.05-4.15 (2H, m), 4.40-4.60 (1H, m), 5.80-6.20 (2H, m).

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 33884-43-4.

Reference:
Patent; Shin-Etsu Chemical Co., Ltd.; US6515149; (2003); B2;,
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. 615-36-1, name is 2-Bromoaniline, This compound has unique chemical properties. The synthetic route is as follows., Safety of 2-Bromoaniline

In a 250 mL round bottom flask, 4.0 g (23.3 mmol) of 2-bromoaniline, 16.1 g (116.5 mmol) of anhydrous potassium carbonate, 7.3 mL (116.5 mmol) of methyl iodide (CH3I) and 50 mL of acetonitrile (MeCN) were added and heated. Up to 70 C.After stirring at 70 C for 18 h, the reaction mixture was cooled to room temperature.It was extracted with 100 mL of deionized water and 100 mL of diethyl ether. After the organic phase is separated,The aqueous phase was washed with 3 x 50 mL diethyl ether. The combined organic phase was washed with 5 x 50 mL of saturated brine.The organic phase was then dried over anhydrous magnesium sulfate. Next, the volatile component in the organic phase was distilled off under reduced pressure to give a crude material. The crude product was separated by silica gel column chromatography to yield 2.7 g of pale yellow oily liquid.The eluent was diethyl ether / hexane (5 / 95 v / v), yield 69%. Relevant characterization data is consistent with the literature reported above.

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 615-36-1.

Reference:
Patent; Hubei University; Liu Li; Chen Bulin; (14 pag.)CN108586536; (2018); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Synthetic Route of 1435-51-4, These common heterocyclic compound, 1435-51-4, name is 1,3-Dibromo-5-fluorobenzene, 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.

According to the reaction formula (2), the specific steps are: in a nitrogen atmosphere,Tris (dibenzylideneacetone) dipalladium (0.4mmol), tri-tert-butylphosphorus (1.2mmol),1-Fluoro-3,5-dibromobenzene (10 mmol) and diphenylamine (22 mmol) were dispersed in anhydrous toluene (80 mL), heated to reflux (110 C.) and reacted at this temperature for 16 h. After the reaction system is cooled to room temperature, the reaction solution is diluted, and the diluted reaction solution is suction-filtered with a Buchner funnel covered with silica gel, and the solution is concentrated at a low pressure, and then a mixture of dichloromethane and n-hexane is used in a volume ratio of 1: 1. Silica gel column chromatography was performed as the eluent to obtain di-tertiary amine compound 1a in a yield of 94%.

The synthetic route of 1435-51-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Beijing University Shenzhen Sheng Yuan; Meng Hong; Shi Ming; Sun Yue; (24 pag.)CN110790782; (2020); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Reference of 583-75-5, 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. 583-75-5 name is 4-Bromo-2-methylaniline, 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.

Step A: ammonium tetrafluoroborate (20.97 g, 200 mmol) was dissolved in aqueous acetic acid (500 ML AcOH/250 ML water) and cooled to 0 C. 2-Methyl-4-bromoaniline (18.61 g, 100 mmol) and 42 ML of aqueous concentrated HCl (36% w/w, 12N, 500 mmol) were sequentially added.The mixture was stirred for 20 minutes at 0 C. and NaNO2 (7.59 g, 110 mmol) was added.The reaction was stirred for 1 hour at 0 C. and warmed to room temperature.After 16 hours at room temperature, the mixture was concentrated under reduced pressure and the residue was azeotroped with toluene and dried under high vacuum.The solid was suspended in 500 ML of CHCl3 and KOAc (12.76 g, 130 mmol) and 18-crown-6 (7.93 g, 30 mmol) were added.The reaction was stirred for 1.5 hours at room temperature.The mixture was washed with water, dried over anhydrous MgSO4, filtered through Celite and concentrated under reduced pressure to provide 30 g of 5-bromo-1H-indazole (compound 2f) as a tan solid.The crude material was used without further purification.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 4-Bromo-2-methylaniline, and friends who are interested can also refer to it.

Reference:
Patent; Munson, Mark; Rizzi, James; Rodriguez, Martha; Kim, Ganghyeok; US2004/176325; (2004); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Some common heterocyclic compound, 452-74-4, name is 1-Bromo-2-fluoro-4-methylbenzene, molecular formula is C7H6BrF, 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. Quality Control of 1-Bromo-2-fluoro-4-methylbenzene

1-Bromo-4-(bromomethyl)-2-fluorobenzene: In a flame dried round-bottomed flask equipped with a magnetic stir bar and under inert atmosphere (N2), a solution of commercially available 1-bromo-2-fluoro-4-methylbenzene (1.37 mL, 106 mmol) in AcCN (25 mL) was treated with /V-bromosuccinimide (2.83 g, 15.9 mmol) and the reaction mixture was heated to 80 C before to add benzoyl peroxide (2.73 mg, 8.46 mmol) and the reaction mixture was stirred for 1.5 h at 80 C. The reaction mixture was partitioned between water (30 mL) and EA (20 mL). The org. layer was washed with brine, dried over MgS04, filtered, and the solvent was removed under reduced pressure. Purification of the residue by FC (1 : 19? 1 : 10 EA/hept) gave the title compound as yellow oil: TLC: rf (1 :10 EA/hept) = 0.58. LC-MS-conditions 07: tR = 0.91 min.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 452-74-4, its application will become more common.

Reference:
Patent; ACTELION PHARMACEUTICALS LTD; CORMINBOEUF, Olivier; CREN, Sylvaine; LEROY, Xavier; POZZI, Davide; WO2015/19325; (2015); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Adding a certain compound to certain chemical reactions, such as: 586-61-8, name is 1-Bromo-4-isopropylbenzene, 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 586-61-8, name: 1-Bromo-4-isopropylbenzene

1.07 g of 0.01 mol of 3-methylaniline, 1.98 g of 0.01 mol of 4-bromoisopropylbenzene, and 3.1 g of sodium t-butoxide were added to a 100 ml three-necked flask, dissolved in 30 ml of toluene solution, and then 0.1 g of pd2 was added under nitrogen atmosphere. (dba) 3, 0.67 g of 10% tri-tert-butylphosphine, heating at 10 C, stirring for 3 hours, the reaction is complete, adding 25 ml of toluene, 25 ml of water, liquid separation, adding the organic phase column to silica gel spin-drying, column chromatography (solvent Ethyl acetate / petroleum ether = 1:20),The column was spun dry to give 1.7 g of white intermediate A2-1, yield 76%.

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-isopropylbenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Beijing Dingcai Technology Co., Ltd.; Gu’an Dingcai Technology Co., Ltd.; Fan Hongtao; Tian Lei; Ren Xueyan; Zhang Xianghui; (35 pag.)CN108129431; (2018); A;,
Bromide – Wikipedia,
bromide – Wiktionary