Category: 314084-61-2

Adding a certain compound to certain chemical reactions, such as: 314084-61-2, name is 2-Bromo-1,3-diethyl-5-methylbenzene, 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 314084-61-2, name: 2-Bromo-1,3-diethyl-5-methylbenzene

Under a nitrogen atmosphere and at normal pressure, 14 g of malonic acid dinitrile dissolved in 7 ml of 1-methyl-2-pyrrolidone are added dropwise in the course of 30 minutes, at from 20 to 25C, to a mechanically stirred mixture of 64 g of sodium carbonate in 200 mi of 1-methyl-2-pyrrolidone. The reaction mixture is heated to 100C and 45.5 g of 2-bromo- 1, 3-diethyl-5-methylbenzene are added, after which the mixture is heated to 120C. At that temperature, a mixture of 0.26 g of TRIPHENYLPHOSPHINE, 0.21 g of a commercially available palladium (LI) chloride solution in concentrated hydrochloric acid (20% Pd content corresponding to 0.071 g of PALLADIUM (II) CHLORIDE in 0.142 g of concentrated hydrochloric acid) and 19.5 g of 1-methyl-2-pyrrolidone is added. The reaction mixture is stirred for from 2 to 3 hours at from 125 to 140C. A gas chromatogram of a sample (1 ml of reaction mixture partitioned between 2 ML of 1 N hydrochloric acid and 2 ml of tert-butyl methyl ether) shows that the product (2-(2, 6-DIETHYL-4-METHYLPHENYL) MALONIC acid dinitrile) has not formed.

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; SYNGENTA PARTICIPATIONS AG; WO2004/50607; (2004); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Application of 314084-61-2, A common heterocyclic compound, 314084-61-2, name is 2-Bromo-1,3-diethyl-5-methylbenzene, molecular formula is C11H15Br, 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.

Dihydro-1H-pyrazolo[1,2-d][1,4,5]oxadiazepine-7,9(2H,8H)-dione (3.4 g, 20 mmol) at 20 C Soluble in 40mL dimethylformamide,And added 2,6-diethyl-4-methylbromobenzene (4.09 g, 18 mmol) andPd(PPh3)2Cl2 (1.26 g, 1.8 mmol) was then stirred at 135 C for 6 hours. After cooling the above reaction system to room temperature, 200 mL of ethyl acetate and 200 mL of diethyl ether were added, and the reaction mixture was poured into a suction filter.100 mL of water and 100 mL of dichloromethane were added to the filtered residue.Acidified with hydrochloric acid. The organic phase was separated, dried and concentrated by evaporation.The residue was chromatographed on silica gel column (ethyl acetate / petroleum ether = 2:1 (V/V))8-(2,6-Diethyl-4-methylphenyl)tetrahydropyrazolo[1,2-d][1,4,5]oxazepine-7,9(2H,8H) -dione4.72 g, yield 82.9%.

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; Lanzhou Fine Chemical High Technology Development Corporation; Gansu Chemical Institute Co., Ltd.; Liu Rong; Wang Xiaoxia; Ji Pengyan; Wei Wanlei; He Kaiyu; Liu Yunli; (9 pag.)CN108864144; (2018); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Adding a certain compound to certain chemical reactions, such as: 314084-61-2, name is 2-Bromo-1,3-diethyl-5-methylbenzene, 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 314084-61-2, Product Details of 314084-61-2

In a 250 mL four-necked reaction flask equipped with a stirrer, thermometer, condenser,32.0 g (0.2 mol)Diethyl malonate, 16 g (0.4 mol) of sodium hydroxide and 100 mL of N-methylpyrrolidone. (0.11111) 2,6-diethyl-4-methyl bromobenzene and 1.28 cuprous bromide were added to a solution of 120 to 130 C for 10 h. Cool, then remove the solvent under negative pressure at 0.095 MPa, 90 C, add 200 g of 7K, adjust the pH to 3 with hydrochloric acid, extract with 3 x 80 mL of ethyl acetate, wash with 3X, 150 mL water, 1 OmL was calcined and crystallized by filtration, washed with n-hexane to give 22.9 g of a pale yellow solid in 75% yield.sodium hydroxideDefinitions of sodium hydroxidenouna strongly alkaline white deliquescent compound used in many industrial processes, e.g., the manufacture of soap and paper.Primary alkaline batteries use sodium hydroxide or potassium hydroxide as the electrolyte.See alsosodium, hydroxideGoogle Translate for Business:Translator ToolkitWebsite Translator

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2-Bromo-1,3-diethyl-5-methylbenzene, and friends who are interested can also refer to it.

Reference:
Patent; Wuhan Institute of Technology; Liu Anchang; Dong Yuanhai; Yu Yu; Zheng Yiqian; Wang Yanlu; (10 pag.)CN106928253; (2017); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Synthetic Route of 314084-61-2,Some common heterocyclic compound, 314084-61-2, name is 2-Bromo-1,3-diethyl-5-methylbenzene, molecular formula is C11H15Br, 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.

21.5 g of sodium ethanolat and 150 g of 1-methyl-2-pyrrolidone are mechanically stirred under a nitrogen atmosphere and at normal pressure. 7.3 g of malonic acid dinitrile are added thereto in portions. 58 g of diluent are distilled off at from 100 to 120C under reduced pressure (from 20 to 30 mbar). Under a nitrogen atmosphere and at normal pressure, 22.7 g of 2-bromo-1, 3-diethyl-5-methylbenzene are added at 110C. The reaction mixture is heated to 125C. At that temperature, a mixture of 0.13 g of TRIPHENYLPHOSPHINE, 0.1 g of a commercially available palladium (lI) chloride solution in concentrated hydrochloric acid (20% Pd content corresponding to 0.035 g of PALLADIUM (II) CHLORIDE in 0.071 g of concentrated hydrochloric acid) and 9.6 g of 1-methyl-2-pyrrolidone is added. The reaction mixture is heated at from 120 to 130C for 1 hour. A mixture of 0.13 g of triphenylphosphine, 0.1 g of a commercially available palladium (II) chloride solution in concentrated hydrochloric acid (20% Pd content corresponding to 0.035 g of palladium (li) chloride in 0.071 g of concentrated hydrochloric acid) and 9.6 g of 1-methyl-2-pyrrolidone is again added. The reaction mixture is stirred for 2 hours at from 120 to 130C. A gas chromatogram of a sample (1 ml of reaction mixture partitioned between 2 ml of 1 N hydrochloric acid and 2 ml of tert-butyl methyl ether) shows that the product (2- (2, 6-diethyl- 4-methylphenyl) malonic acid dinitrile) has not formed.

The synthetic route of 314084-61-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SYNGENTA PARTICIPATIONS AG; WO2004/50607; (2004); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Synthetic Route of 314084-61-2,Some common heterocyclic compound, 314084-61-2, name is 2-Bromo-1,3-diethyl-5-methylbenzene, molecular formula is C11H15Br, 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.

Under a nitrogen atmosphere, 14.2 g of malonic acid dinitrile are added at normal pressure and room temperature to a mixture of 48 g of a 50% aqueous solution of sodium hydroxide and 300 g of 1-methyl-2-pyrrolidone. The reaction mixture is heated to from 60 to 100C, and 98 g of diluent are distilled off under reduced pressure (from 25 to 30 mbar). Under a nitrogen atmosphere, 45.5 g of 2-bromo-1, 3-diethyl-5-methylbenzene are added at normal pressure. The reaction mixture is then heated to 130C with stirring. At that temperature, a mixture of 0.26 g of TRIPHENYLPHOSPHINE, 0.2 g of a commercially available palladium (lI) chloride solution in concentrated hydrochloric acid (20% Pd content corresponding to 0.071 g of Pd (LI) chloride and 0.142 g of concentrated hydrochloric acid) and 19.5 g of 1-methyl-2-pyrrolidone is added. The mixture is stirred at from 125 to 130C for a further 3 hours and then 199 g of diluent are distilled off at reduced pressure (from 20 to 25 mbar) at from 90 to 100C. After cooling to room temperature, the reaction mixture is added to 126 g of water. 4.5 g of Hyflo (Celite) are added thereto, and the mixture is stirred for 30 minutes at 40C before being filtered. The filter cake is washed with 114 g of water. Following the addition of 45 g of 32% hydrochloric acid to the filtrate (a pH value of less than 5 is then established), the precipitated solid is filtered off and washed with 120 g of water. After drying, 42.8 G (content 97.3%, yield 98.0%) of 2- (2, 6-diethyl-4- METHYLPHENYL) MALONIC acid dinitrile having a melting point of from 79 to 82C are obtained.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2-Bromo-1,3-diethyl-5-methylbenzene, its application will become more common.

Reference:
Patent; SYNGENTA PARTICIPATIONS AG; WO2004/50607; (2004); 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 314084-61-2 as follows. Recommanded Product: 2-Bromo-1,3-diethyl-5-methylbenzene

Step 2: Set up a 1000mL four-neck bottle, thermometer,Three-way nitrogen ball device, the system uses an oil pump to pump vacuum and use nitrogenAfter gas replacement for three times, under nitrogen protection,Add 100 mL of tetrahydrofuran to the system.2,6-Diethyl-4methylbromobenzene 20g (molecular weight 227.1, 0.088mol), cooled to -60 C, control the temperature of the reaction solution between -50 C and -60 C, slowly add 528 mL 1 mol / L positive Butyl lithium in n-hexane solution (0.528 mol),After the addition was completed, the temperature was kept at -50 C to -60 C for 1 h.16.49 g of 2-bromoethanol (molecular weight 124.96, 0.132 mol) was slowly added dropwise at -50 C to -60 C, and the reaction was kept after the addition.0.5h. The reaction solution was quenched with 50 mL of 1 mol/L diluted hydrochloric acid and extracted twice with 50 mL of ethyl acetate.To dryness, 16.3 g of a colorless oil was obtained. After 10 min, the oil was turned to white solid.

According to the analysis of related databases, 314084-61-2, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Jiangsu Zhongqi Technology Co., Ltd.; Bu Long; Zhang Pu; Qian Ziwei; Gao Miao; Wang Fengyun; Hou Yuanchang; (10 pag.)CN109651068; (2019); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Reference of 314084-61-2, These common heterocyclic compound, 314084-61-2, name is 2-Bromo-1,3-diethyl-5-methylbenzene, 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) Under a nitrogen atmosphere and at normal pressure, 7 g of malonic acid dinitrile dissolved in 3.5 ml of 1-methyl-2-pyrrolidone are added dropwise in the course of 30 minutes, at from 20 to 30C, to a mechanically stirred mixture of 12 g of sodium hydroxide (pellets) in 150 ml of dimethyl sulfoxide. Evacuation to from 10 to 30 mbar is carried out, and 79.1 g of solvent are distilled off at from 80 to 100C. After establishing normal pressure, 24 g (content 94.9%) of 2-bromo-1, 3-diethyl-5-methylbenzene are added, and the reaction mixture is heated to 130C. At that temperature, a mixture of 0.13 g of TRIPHENYLPHOSPHINE, 0.1 g of a commercially available palladium (II) chloride solution in concentrated hydrochloric acid (20% Pd content corresponding to 0.035 g of palladium (li) chloride in 0.071 g of concentrated hydrochloric acid) and 9.6 g of 1-methyl-2-pyrrolidone is added. The reaction mixture is stirred for from 2 to 3 hours at from 125 to 140C. A further 59.5 g of solvent are distilled off at from 20 to 60 mbar. 1.5 g of Hyflo and 75 ml of water are added to the residue which has been cooled to 50C. The reaction mixture is stirred vigorously for 10 minutes and then clarified by filtration over Hyflo. The filter is then washed with 50 ml of water. 23.3 g of 32% hydrochloric acid are added to the filtrate in the course of from 60 to 80 minutes, at from 20 to 25C, during the course of which the product crystallises out and the pH value falls to from 4.0 to 4.5. Suction filtration is carried out, followed by washing with 100 ml of water (divided into 2 portions). The product is dried in a vacuum drying cabinet for 16 hours at from 100 to 250 mbar. 20.6 g (content 97.9% ; yield 95. 1%) of 2- (2, 6-diethyl-4-methylphenyl) malonic acid dinitrile are obtained.

The synthetic route of 314084-61-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SYNGENTA PARTICIPATIONS AG; WO2004/50607; (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. 314084-61-2, name is 2-Bromo-1,3-diethyl-5-methylbenzene, A new synthetic method of this compound is introduced below., Safety of 2-Bromo-1,3-diethyl-5-methylbenzene

Under a nitrogen atmosphere, 14.2 g of malonic acid dinitrile are added at normal pressure and room temperature to a mixture of 67.3 g of 50% potassium hydroxide solution and 300 mi of 1-methyl-2-pyrrolidone. The reaction mixture is heated to from 60 to 100C, and 106 g of diluent are distilled off at reduced pressure (from 20 to 30 mbar). Under a nitrogen atmosphere and at normal pressure, 45.5 g of 2-bromo-1, 3-diethyl-5-methylbenzene are added. The reaction mixture is then heated to 120C with stirring, At that temperature, a mixture of 0.26 g of TRIPHENYLPHOSPHINE, 0.2 g of a commercially available palladium (LI) chloride solution in concentrated hydrochloric acid (20% Pd content corresponding to 0.071 g of palladium (II) chloride and 0.142 g of concentrated hydrochloric acid) and 19.5 g of 1-METHYL-2-PYRROLIDONE is added. Stirring is carried out at from 120 to 125C FOR 1 hour, and then a mixture of 0.26 g of triphenylphosphine, 0.2 g of a commercially available PALLADIUM (II) chloride solution in concentrated hydrochloric acid (20% Pd content corres- ponding to 0.071 g of palladium (li) chloride and 0.142 g of concentrated hydrochloric acid) and 19.5 g of 1-METHYL-2-PYRROLIDONE is again added. The reaction mixture is stirred for 3 hours at from 120 to 125C, and then a further 237 g of diluent are distilled off at reduced pressure (from 20 to 30 mbar) and at from 80 to 120C. After cooling the reaction mixture to 45C, 100 mi of toluene and 220 g of water are added and intensive stirring is carried out for 15 minutes. The two-phase mixture is transferred to a separating funnel in order to be separated. The organic phase is discarded. The aqueous phase is isolated and and 43.4 g of material are distilled off at reduced pressure (from 250 to 300 mbar) and at from 70 to 110C. 48.5 g of 32% hydrochloric acid are added in the course of from 60 to 80 minutes to the distillation sump, during the course of which the product crystallises out and the pH value falls to from 4.0 to 4.5. Suction filtration is carried out followed by washing with 130 ml of water (divided into 2 portions). The product is dried in a vacuum drying cabinet for 16 hours at from 100 to 250 mbar. 37.2 g (content 97.7% ; yield 85.7%) of 2- (2, 6-diethyl-4- methylphenyl) malonic acid dinitrile are obtained.

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; SYNGENTA PARTICIPATIONS AG; WO2004/50607; (2004); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

These common heterocyclic compound, 314084-61-2, name is 2-Bromo-1,3-diethyl-5-methylbenzene, 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. Formula: C11H15Br

Under a nitrogen atmosphere, 13.9 G of malonic acid dinitrile are added at normal pressure and room temperature to 20.4 g of pulverulent sodium hydroxide in 240 g of 1-methyl-2- pyrrolidone. After the addition of 45.5 g of 2-bromo-1, 3-diethyl-5-methylbenzene, the reaction mixture is heated to 125C with stirring. At that temperature, a mixture of 1.3 g of triphenylphosphine, 1.06 g of a commercially AVAILABLE PALLADIUM (II) chloride solution in concentrated hydrochloric acid (20% Pd content corresponding to 0.354 g of Pd (LI) chloride and 0.708 g of concentrated hydrochloric acid) and 97.6 g of 1-methyl-2-pyrrolidone is added. Stirring is carried out for a further 3 hours at from 125 to 130C, and 283 g of diluent are distilled off at reduced pressure (from 17 to 100 mbar). After cooling to room temp- erature, the reaction mixture is added to 70 g of water. Following the addition of 38 g of concentrated hydrochloric acid (a pH value of less than 5 is then established), the precipitated solid is filtered off and washed with 60 g of water. After drying, 42.4 G of 2- (2, 6- diethyl-4-methylphenyl) malonic acid dinitrile (content 92.3%, yield 92.3%) having a melting point of from 74 to 78C are obtained.Example P4: Preparation of 2- (2, 6-diethyl-4-methylphenyl) malonic acid dinitrile Under a nitrogen atmosphere and at normal pressure, 14 g (217 MMOL) of malonic acid dinitrile dissolved in 7 ml of 1-methyl-2-pyrrolidone are added dropwise in the course of 30 minutes, at from 20 to 25C, to a mechanically stirred mixture of 24.1 g (600 MMOL) of sodium hydroxide (pellets) in 300 ml of 1-methyl-2-pyrrolidone. Evacuation to from 10 to 30 mbar is carried out and, at from 80 to 100C, 113 g of solvent are distilled off. After establishing normal pressure, 48 g (content 94.9% ; 200 MMOL) of 2-bromo-1, 3-DIETHYL-5- METHYLBENZENE are added and the reaction mixture is heated to 130C. At that temperature, a mixture of 0.26 g (1 MMOL) of triphenylphosphine, 0.21 g of a commercially available palladium (li) chloride solution in concentrated hydrochloric acid (20% Pd content corresponding to 0.071 g (400 UMOL) of PALLADIUM (II) CHLORIDE in 0.142 g of concentrated hydrochloric acid) and 19.5 g of 1-methyl-2-pyrrolidone is added. The reaction mixture is stirred for from 2 to 3 hours at from 125 to 140C, nitrogen being introduced below the surface. A further 165 g of solvent are distilled off at from 20 to 60 mbar. 2.3 g of Hyflo and 150 ml of water are added to the residue which has been cooled to 50C. The reaction mixture is stirred vigorously for 10 minutes and then clarified by filtration over Hyflo. The filter is subsequently washed with 55 ml of water. The combined aqueous phases are extracted once with 91 g of toluene. The organic phase is separated off and discarded. 30 g of toluene/water are distilled off from the aqueous phase at from 20 to 70C and from 200 to 250 mbar. At from 20 to 25C there are added to the distillation sump, in the course of from 60 to 80 minutes, 45.7 g of 32% hydrochloric acid, during the course of which the product crystallises out and the pH value falls to from 4.0 to 4.5. Filtration with suction is carried out, followed by washing with 120 ml of water (divided into 2 portions). The product is dried in a vacuum drying cabinet for 16 hours at from 100 to 250 mbar. 42.2 g (content 98.2% ; yield 97.6%) of 2- (2, 6-DIETHYL-4-METHYLPHENYL) MALONIC acid dinitrile are obtained.

The synthetic route of 2-Bromo-1,3-diethyl-5-methylbenzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SYNGENTA PARTICIPATIONS AG; WO2004/50607; (2004); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Electric Literature of 314084-61-2,Some common heterocyclic compound, 314084-61-2, name is 2-Bromo-1,3-diethyl-5-methylbenzene, molecular formula is C11H15Br, 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.

Add 9.8g to a 250mL four-necked flask at room temperature under nitrogen.Potassium hydroxide and 150 mL of 1-methyl-2-pyrrolidone, then add 6.5 g of malononitrile, and heat up to 80-100 C to distill off 40 mL of solution.12.4g of 2,6-diethyl-4-methylbromobenzene was added under normal pressure.Stir and warm the reaction mixture to 125 C.Add 0.14g of cuprous iodide, 0.29g of 3,4,7,8-tetramethyl-1,10-phenanthroline, react at 130 C for 5 hours, cool down, distill off the solvent under reduced pressure, and add 100 g to the residue. Water, adjust the pH to 3-4 with hydrochloric acid to precipitate a solid, filter, solid wash with water to neutral, and dry to obtain 2,6-diethyl-4-methylphenylmalononitrile 10.7 g, yield 92.7% .

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2-Bromo-1,3-diethyl-5-methylbenzene, its application will become more common.

Reference:
Patent; Zhejiang Zhongshan Chemical Group Co., Ltd.; Wu Tongwen; Yang Zhi; Liu Zhigang; Chen Lu; Lin Bingan; Zhang Lei; (6 pag.)CN109912457; (2019); A;,
Bromide – Wikipedia,
bromide – Wiktionary