Category: 31599-61-8

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. 31599-61-8, name is 4-Iodo-1,2-dimethylbenzene, A new synthetic method of this compound is introduced below., Quality Control of 4-Iodo-1,2-dimethylbenzene

General procedure: A mixture containing styrene (3.5 mmol), aryl halide (3.5 mmol), the palladium complex [(L)PdCl] (0.001 mmol) and potassium carbonate (8.0 mmol) in methanol (10 ml) were heated to reflux for 4 h. After evaporation of solvent the product was poured into water and extracted with diethyl ether. The ether solution was dried over Na2SO4 and filtered. The ether solution were passed through silica column (60-120 mesh), the complex remain trapped. After extraction of desired compound complex was extracted using dichloromethane. Upon evaporation of the ether, solid of pure products were obtained. The yields of the products obtained from all the reactions were determined after isolation and characterized by 1H NMR spectra.

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:
Article; Pattanayak, Poulami; Pratihar, Jahar Lal; Patra, Debprasad; Lin, Chia-Her; Paul, Sobhana; Chakraborty, Kausiki; Polyhedron; vol. 51; 1; (2013); p. 275 – 282;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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 31599-61-8 as follows. SDS of cas: 31599-61-8

General procedure: In a typical experiment the catalyst (containing 2.8 lmol Pd) was placed in a stainless steel autoclave. The aryl iodide (0.2 mmol), amine (0.5 mmol), base (35 ll, 0.25 mmol) and solvent (1 ml) were transferred into it under an inert atmosphere. It was charged with carbon monoxide (30 bar or 5 bar) and heated with stirring in an oil bath at 100 C or 120 C. After cooling to room temperature the catalyst was removed by filtration and was reused without further purification if the product was soluble in the solvent. In other cases, the solid material was washed by acetone and the catalyst was dried in vacuo prior to reuse. The reaction mixture was analyzed by gas chromatography.

According to the analysis of related databases, 31599-61-8, the application of this compound in the production field has become more and more popular.

Reference:
Article; Urban, Bela; Skoda-Foeldes, Rita; Phosphorus, Sulfur and Silicon and the Related Elements; vol. 194; 4-6; (2019); p. 302 – 306;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 31599-61-8, A common heterocyclic compound, 31599-61-8, name is 4-Iodo-1,2-dimethylbenzene, molecular formula is C8H9I, 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 2M solution of i-PrMgC1 in THF (0.275 liter, 0.55M) and THF (1.0 liter) was introduced to a 2 liter flask at 12C. Intermediate 1 (121.8g, 0.525M) was added dropwise during 20 mm. The mixture was stirred at 12-15C for 3 hrs.Intermediate 2 (84.6g, 0.25M) was added in small portions without cooling during 30 mm, with a temperature rise to 25C, to give a light brown solution. The solution was stirred for 2.Shrs at 15C and added to aqueous solution of NH4C1 (1 17g in 0.7 liter water) during 10 mm at 5C. PE (1.6 liter) was added during 5 mm and the mixture stirred for extra 25 mm.Precipitated solid filtered on Buechner funnel and then re-slurred with mixture of MTBE (400 ml), water (600 ml) and PE (200 ml). Then the solid was filtered on Buechner funnel and re-slurred with MeOH (700 ml) at 60C for 10 mm, cooled to 20C with cold water bath and filtered again on Buechner funnel. The solid product was dried in an air oven at 45C for 2 hrs to give 112 g of intermediate 3 as a white solid with a yield of 89.9%.

The synthetic route of 31599-61-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; CLEXIO BIOSCIENCES LTD.; FRENKEL, Anton; IOFFE, Vladimir; (54 pag.)WO2020/16827; (2020); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 31599-61-8, These common heterocyclic compound, 31599-61-8, name is 4-Iodo-1,2-dimethylbenzene, 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.

General procedure: To a stirred solution of Pd cNPs/C Fe3O4 (20 mg, 0.73 mol %) and DMF (3 mL) in a Schlenk tube with a teflon stopcock, iodobenzene (0.5 mmol), tri-n-butylphenylstanane (0.6 mmol) and K2CO3 (1.5 mmol) are added, sealed and heated at 100 oC for 10 h. After completion of the reaction, the catalyst is separated by an external magnet. After removal of catalyst, water was added to the solution and extracted with ethylacetate. The organic phase is dried over anhydrous Na2SO4. After evaporation of the solvents, the residue is subjected to column chromatography over silica gel (60-120 mesh), eluting with pet ether to afford the desired product. The biphenyl products were confirmed by 1H and 13C-NMR. The spectral data and spectra are shown in supporting information (Figure S5-S18). This procedure was followed for all the reactions listed in Table 2.

The synthetic route of 31599-61-8 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Kumar, Basuvaraj Suresh; Anbarasan, Rajagopal; Amali, Arlin Jose; Pitchumani, Kasi; Tetrahedron Letters; vol. 58; 33; (2017); p. 3276 – 3282;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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 31599-61-8 as follows. SDS of cas: 31599-61-8

General procedure: To the catalyst (1.0mol%) dissolved in 10ml THF in a 25ml round-bottom flask, aryl halide (1.0mmol), phenyl boronic acid (1.2mmol) and K2CO3 (2.0mmol) were all added. The mixture was stirred at refluxing temperature for 4h. After completion of the reaction, the mixture was evaporated to dryness, water was added and the product was extracted with dichloromethane. The organic layer was washed with brine, dried over Na2SO4, filtered, passed through a silica column (60-120 mesh), where the complex remained trapped. Upon removal of the solvent, pure solid products were obtained. The yields of the products obtained (based on the aryl halides) from all the reactions were determined after isolation, and the products were characterized by 1H NMR spectra and melting points by a comparison with the literature data.

According to the analysis of related databases, 31599-61-8, the application of this compound in the production field has become more and more popular.

Reference:
Article; Pratihar, Jahar Lal; Mandal, Paritosh; Lin, Chia-Her; Lai; Mal, Dasarath; Polyhedron; vol. 135; (2017); p. 224 – 230;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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. 31599-61-8, name is 4-Iodo-1,2-dimethylbenzene, A new synthetic method of this compound is introduced below., name: 4-Iodo-1,2-dimethylbenzene

General procedure: In an oven dried round bottomed flask a mixture of phenyl boronic acid (0.244g, 2.0mmol), aryl halide (2.0mmol), the palladium complex [Pd(OL1)]4 (0.002mmol) and potassium carbonate (0.145g, 2.5mmol) in THF (10cm3) was heated to reflux for 2h, as mentioned in Table 2. After the reaction was completed, the solvent was evaporated and the reaction mixture was extracted with diethyl ether. The ether solution was dried over Na2SO4 and filtered. The ether solution, containing the reaction mixture, was passed through a 30.48cm silica column (60-120 mesh), the complex was not separated out and it remained trapped in the column. After the desired compound was extracted from the column, the complex was extracted using dichloromethane. The unchanged complex was used twice. After evaporation of the ether, solids of the pure products were obtained. The yields of the products obtained from all the reactions were determined after isolation, and the products were characterized by 1H NMR spectra.

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:
Article; Pattanayak, Poulami; Pratihar, Jahar Lal; Patra, Debprasad; Lin, Chia-Her; Chattopadhyay, Surajit; Polyhedron; vol. 63; (2013); p. 133 – 138;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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 31599-61-8 as follows. SDS of cas: 31599-61-8

General procedure: A 10 mL Schlenk tube was charged with 2-phenylindole 1a (193.2 mg, 1.0 mmol), CuI (10 mol%, 19.0 mg, 0.1 mmol) and K3PO4 (424 mg, 2.0 mmol). The Schlenk tube was evacuated and filled with N2 (this procedure was repeated three times), and then toluene (2.0 mL), DMEDA (20 mol%, 17.6 mg, 0.2 mmol) and iodobenzene 2a (244.8 mg, 1.2 mmol) were added. The resulting mixture was stirred at 110 C for 24 h. After cooling to room temperature, the reaction mixture was quenched and extracted with ethyl acetate (10 mL × 3). The organic extracts were combined, dried over Na2SO4 and concentrated under reduced pressure, and then purified by silica gel chromatograph (petroleum ether) to yield the desired product as a white solid (245.1 mg, 91% yield). The data of compounds 3a-q can be found in Supporting information.

According to the analysis of related databases, 31599-61-8, the application of this compound in the production field has become more and more popular.

Reference:
Article; Liu, Wei; Han, Li-Ya; Liu, Rui-Li; Xu, Li-Ge; Bi, Yan-Lan; Chinese Chemical Letters; vol. 25; 9; (2014); p. 1240 – 1243;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 31599-61-8, 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. 31599-61-8 name is 4-Iodo-1,2-dimethylbenzene, 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.

General procedure: Amide derivatives (0.2 mmol), 4-methoxy iodobenzene (3 equiv.), Pd(OAc)2 (10 mmol%), C6H13COOAg (2 equiv.) were combined in o-xylene (1 mL) in a 10mL vial. The vial was sealed with a Teflon lined cap, and the reaction was stirred in 120 C oil bath for 24 hours without an inert gas atmosphere. After cooled to room temperature, the mixture was extracted with ethyl acetate (3 x 10mL). The residue was purified by silica-gel column chromatography to afford the corresponding product.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 4-Iodo-1,2-dimethylbenzene, and friends who are interested can also refer to it.

Reference:
Article; Yan, Xufei; Long, Rongrong; Luo, Feihua; Yang, Li; Zhou, Xiangge; Tetrahedron Letters; vol. 58; 1; (2017); p. 54 – 58;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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. 31599-61-8, name is 4-Iodo-1,2-dimethylbenzene, This compound has unique chemical properties. The synthetic route is as follows., Product Details of 31599-61-8

4-Iodo-1,2-dimethylbenzene (12.9 g, 55.6 mmol) was charged into the reaction flask with dimethyl sulfoxide-d6 (D6-DMSO)(60 ml, 857 mmol) followed by sodium tert-butoxide (1.8 g, 18.75 mmol). This mixture was degassed with nitrogen then was stirred at 65 C. for 18 hours. The reaction was cooled down and quenched with 75 mL of D2O. This mixture was stirred at room temperature (22 C.) for 45 minutes. The mixture was then diluted with 200 mL of water and was extracted with 3×70 mL of dichloromethane (DCM). These extracts were dried over magnesium sulfate, filtered and concentrated under vacuum. The crude residue was subjected to column chromatography on silica gel eluted with DCM/heptanes 95/5 (v/v). Pure fractions were combined and concentrated under vacuum yielding 4-iodo-1,2-bis(methyl-d3)benzene (12.1 g, 50.8 mmol, 91% yield).

According to the analysis of related databases, 31599-61-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Universal Display Corporation; TSAI, Jui-Yi; DYATKIN, Alexey Borisovich; YEAGER, Walter; XIA, Chuanjun; (238 pag.)US2018/102487; (2018); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 31599-61-8, name is 4-Iodo-1,2-dimethylbenzene, belongs to iodides-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 31599-61-8, Quality Control of 4-Iodo-1,2-dimethylbenzene

14 Typical procedure for the preparation of 4,5-disubstituted-1,2,3-(NH)-triazoles (synthesis of 3a): A round-bottom sidearm flask (10 mL) containing PdCl2(PPh3)2 (0.015 mmol) was subjected to the Schlenk-line procedures of evacuation and purging of CO for three cycles. Iodobenzene and 4 equiv Et3N (1.2 mmol) were successively added, and the mixture was stirred at room temperature for 10 min, then 1-hexyne (0.45 mmol) was added, continuously stirred at room temperature for 14 h. Then NaN3 (35.1 mg, 0.54 mmol) and 1 mL DMSO were added to the mixture and the reaction continued at 45 C for 36 h. Following, to the reaction mixture was added water (2 mL), 20% HCl solution (1 mL) and extracted with ether (3 * 10 mL). The combined organic phases were washed with brine (2 * 5 mL), dried over anhydrous MgSO4 and concentrated in vacuo. The residue was subjected to flash column chromatography with hexanes/EtOAc (5/1) as eluent to obtain the desired 3a (56.33 mg, 82% yield). All products gave satisfactory spectroscopic and analytical data.

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-Iodo-1,2-dimethylbenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Li, Na; Wang, Dong; Li, Jihui; Shi, Weilin; Li, Chao; Chen, Baohua; Tetrahedron Letters; vol. 52; 9; (2011); p. 980 – 982;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com