Category: 82998-57-0

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. 82998-57-0, name is 3-Iodo-4-methylbenzoic acid, This compound has unique chemical properties. The synthetic route is as follows., Safety of 3-Iodo-4-methylbenzoic acid

To the flask was added 250 ml of thionyl chloride and 26.2 g of 3-iodo-4-methylbenzoic acid, stirred and heated under reflux for 6 h,After drying under reduced pressure, dry dichloroethane was added and the solvent was removed under reduced pressure.Followed by adding 250 ml of chloroform, 20 ml of diisopropylethylamine,A solution of 24.1 g of 3- (4-methylimidazol-1-yl) -5-trifluoromethylaniline, and the temperature was raised to 60 C for 5 h.After completion of the reaction, the solvent was concentrated under reduced pressure to remove the solvent. Add ethyl acetateEster 200ml dissolved, washed 3 times, dried and concentrated, the resulting solid separation by column chromatography, eluentDichloromethane / methanol = 9, the desired fractions were collected and concentrated to give 28 g of a solid in 57% yield.

According to the analysis of related databases, 82998-57-0, the application of this compound in the production field has become more and more popular.

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. 82998-57-0, name is 3-Iodo-4-methylbenzoic acid, This compound has unique chemical properties. The synthetic route is as follows., Safety of 3-Iodo-4-methylbenzoic acid

Add 2 drops of DMF into 628 mg 3-iodo-4-methylbenzoic acid (2.2 mmol) in 20 mL SOCl2 and reflux for 2 h. After vacuum evaporation of SOCl2, add 6.0 mL anhydrous THF and get the pale yellow solution. Dissolve the product from step 1, 524 mg 5-(4-methyl-1H-imidazol-1-yl)-3-(trifluoromethyl)-benzenamine (2.0 mmol) in 6.0 mL anhydrous THF and add 10 mmol Et3N, and the pale yellow solution prepared previously is added drop wise till it is all added. The reaction mixture rises to room temperature for 1 hr. The reaction was quenched with addition of brine and extracted with EtOAc. The combined extraction organic layers was dried and concentrated under vacuum, the residue was purified through column chromatography to afford 873 mg desired product. (90%)MS (ESI), m/z: 486 (M+ + H+).

According to the analysis of related databases, 82998-57-0, the application of this compound in the production field has become more and more popular.

Electric Literature of 82998-57-0, 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. 82998-57-0, name is 3-Iodo-4-methylbenzoic acid belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To a solution of 3-iodo-4-methylbenzoic acid (628 mg, 2.2mmol) in SOCl2 (20 mL) was added two drops of DMF. After heatingunder reflux for 2 h, the SOCl2 was evacuated, and the residue was dissolved in anhydrous THF (6 mL) to form light yellow solution.

The synthetic route of 3-Iodo-4-methylbenzoic acid has been constantly updated, and we look forward to future research findings.

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. 82998-57-0, name is 3-Iodo-4-methylbenzoic acid, A new synthetic method of this compound is introduced below., HPLC of Formula: C8H7IO2

Thionyl chloride (8.2 ml,112.5 mmol) was added to a solution of 3-iodo-4-methyl-benzoic acid (18.5 g, 75 mmol) In 100 ml of chloroform,The reaction was stirred at 60 C for 16 hours.The solvent was concentrated under reduced pressure,Excessive dichlorosulfoxide with 30 cents Rose to azeotropically remove,To give the product 19.5 g,93% yield,Can be used directly for the next step.

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.

Related Products of 82998-57-0, 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. 82998-57-0, name is 3-Iodo-4-methylbenzoic acid, This compound has unique chemical properties. The synthetic route is as follows.

3-lodo-4-methylbenzoic acid (3.07 g, 0.0117 mol) was added thionyl chloride (10 mL) and refluxed for 2 h. The excess thionyl chloride was carefully removed and the resulting acid chloride was dried in vacuo for 2 h. The residue was then dissolved in DCM (anhydrous, 25 mL) and cooled on ice. To the cooled solution was added 3-(1H-imidazol-1-yl)-5- (trifluoromethyl)aniline 5 (3.46 g, 0.0152mol) in DCM followed by the dropwise addition of diisopropylethylamine (8.2 mL, 0.047 mol). This was stirred at ambient temperature for 21 h. The white solid that separated was filtered and washed with water and dried to provide 4.65 g of product. Additional product could be obtained from the filtrate following concentration and purification by silica gel flash chromatography in EtOAc/hexanes.

The chemical industry reduces the impact on the environment during synthesis 3-Iodo-4-methylbenzoic acid. I believe this compound will play a more active role in future production and life.

Reference:
Patent; ARIAD PHARMACEUTICALS, INC.; WO2007/75869; (2007); A2;,
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 82998-57-0 as follows. Quality Control of 3-Iodo-4-methylbenzoic acid

To a solution of 3-iodo-4-methyl-benzoic acid (10.0 g, 38.2 mmol) in methanol (70 ml) is added concentrated sulfuric acid (0.5 ml). The reaction mixture is heated at 70 C. for 48 hours, cooled to room ambient temperature and then concentrated. After that, ethyl acetate (100 ml) and aqueous NaHCO3 (saturated, 100 ml) solution are added to the residue. The organic layer is separated and washed again with aqueous NaHCO3 (saturated, 100 ml) solution. The organic layer is separated, dried over anhydrous Na2SO4 and concentrated to yield 3-iodo-4-methyl-benzoic acid methyl ester 1. It is used without further purification in the next step. 1H NMR (400 MHz, DMSO-d6) delta 8.31 (s, 1H), 7.87 (d, 1H, J=8.4 Hz), 7.48 (d, 1H, J=8.4 Hz), 3.85 (s, 3H), 3.35 (s, 3H); LC-MS m/z: 277.0 (M+1).

According to the analysis of related databases, 82998-57-0, the application of this compound in the production field has become more and more popular.

Reference:
Patent; IRM LLC; US2009/203666; (2009); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 82998-57-0, 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. 82998-57-0, name is 3-Iodo-4-methylbenzoic acid, This compound has unique chemical properties. The synthetic route is as follows.

To a solution of 3-iodo-4-methylbenzoic acid 5-1 (262mg, 1.0mmol) in dry DCM (10mL) at 0C was added oxalyl chloride (0.13mL, 1.5mmol) and 3 drops of dry DMF. The resulting reaction mixture was stirred at room temperature for 3h, and then the solvent was removed under reduced pressure. The crude product was used directly for the next step without further purification.

The chemical industry reduces the impact on the environment during synthesis 3-Iodo-4-methylbenzoic acid. I believe this compound will play a more active role in future production and life.

Reference:
Article; Liu, Yang; Peng, Xia; Guan, Xiaocong; Lu, Dong; Xi, Yong; Jin, Shiyu; Chen, Hui; Zeng, Limin; Ai, Jing; Geng, Meiyu; Hu, Youhong; European Journal of Medicinal Chemistry; vol. 126; (2017); p. 122 – 132;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 82998-57-0,Some common heterocyclic compound, 82998-57-0, name is 3-Iodo-4-methylbenzoic acid, molecular formula is C8H7IO2, 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.

REFERENCE EXAMPLE 19; 4-Methyl-3-(4,4,5,5-tetramethyl[1 ,3,2]dioxaborolan-2-yl)benzoic acid; To a solution of 3-iodo-4-methylbenzoic acid (3.71 g, 14.2 mmol) in DMF (130 mL), bis(pinacolato)diboron (7.20 g, 28.4 mmol), [1 ,1′-bis(diphenylphosphino) EPO ferrocene]dichloro-palladium (II) (1.04 g, 1.28 mmol) and potassium acetate (6.95 g, 70.9 mmol) were added under argon. The mixture was heated at 80 0C overnight and then allowed to cool to room temperature. The solvent was evaporated and the residue was diluted with water and EtOAc. The phases were separated and the aqueous phase was extracted with EtOAc. The combined organic phases were washed twice with 3N HCI and dried over Na2SO4. The solvent was evaporated and the crude product thus obtained was purified by chromatography on silica gel using hexane-EtOAc mixtures of increasing polarity as eluent, to afford the title compound impurified with starting bis(pinacolato)diboron. The product was slurried in hexane, filtered and dried under vacuum to afford 2.41 g of pure material (yield: 65%). 1H NMR (300 MHz1 CDCI3) delta (TMS): 1.36 (s, 12 H), 2.61 (s, 3 H)1 7.25 (d, J = 8.1 Hz1 1 H), 8.02 (dd, J = 8.1 Hz1 J1 = 2.1 Hz, 1 H)1 8.48 (d, J = 2.1 Hz, 1 H). LC-MS (method 1): tR = 7.57 min; m/z = 261.0 [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 3-Iodo-4-methylbenzoic acid, its application will become more common.

Reference:
Patent; J. URIACH Y COMPANIA S.A.; WO2007/339; (2007); A1;,
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. 82998-57-0, name is 3-Iodo-4-methylbenzoic acid, A new synthetic method of this compound is introduced below., Quality Control of 3-Iodo-4-methylbenzoic acid

To a stirring solution of 3-iodo-4-methylbenzoic acid (60 g, 0.22 mol, 1 eq) in degassed DMF (1400 niL, 23.3 vol.) was charged 4,4,4′,4′,5,5,5′,5′-octamethyl-2,2′-bi-l,3,2- dioxaborolane (81.4 g, 0.32 mol, 1.4 eq) followed by potassium acetate (112 g, 1.14 mole, 5eq) and [1,1 ‘-bis(diphenylphosphino)ferrocene]-dichloropalladium(II) (18.7 g, 0.02 mole, 0. leq). The resulting mixture was placed under a nitrogen atmosphere and was heated to 80 0C with the exclusion of light overnight. The mixture was then concentrated under high vacuum and the residue partitioned between EtOAc and 2M HCl. The mixture was then filtered and the layers separated. The aqueous phase was re-extracted with EtOAc. The combined organics were then washed with brine, dried and evaporated to yield a brown solid that was applied to a silica plug then eluted with 2:1 cyclohexane : ethyl acetate. Fractions were then combined and evaporated to yield a brown foam that was triturated with cyclohexane, collected by filtration then dried in vacuo to yield 4-methyl-3-(4,4,5,5- tetramethyl-l,3,2-dioxaborolan-2-yl)benzoic acid, delta (CDCl3) 8.50-8.49 (IH, d), 8.04-8.02 (IH, dd), 7.27-7.25 (IH, d), 2.61 (3H, s), 1.36 (12H, s).

The synthetic route of 82998-57-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; GLAXO GROUP LIMITED; WO2007/147104; (2007); A2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 82998-57-0,Some common heterocyclic compound, 82998-57-0, name is 3-Iodo-4-methylbenzoic acid, molecular formula is C8H7IO2, 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.

3-iodo-4-methylbenzoic acid (3.2 g, 12.2 mmol) was dispersed in 50 mL of thionyl chloride.The reaction system was heated to 82 C, kept under reflux for 1 hour, and cooled to room temperature.The reaction solution was added to 50 mL of toluene while maintaining slow stirring.Concentrate under reduced pressure to a pale yellow oil.After the concentrate was dissolved in 100 mL of dichloromethane,To this solution was added 3-trifluoromethylaniline (2.3 mL, 18.3 mmol) and diisopropylethylamine (9 mL).The reaction system was stirred at room temperature overnight to precipitate a large amount of white solid.The reaction solution was concentrated under reduced pressure and then evaporated.Washed with saturated ammonium chloride solution and saturated brine,The organic phase was dried over anhydrous magnesium sulfate and concentrated.Purification by silica gel column chromatography to obtain compound 8(3.5 g, 71%) was obtained as a white solid.

The synthetic route of 82998-57-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Shenzhen Ruixi Biological Technology Co., Ltd.; Jiao Zhaodong; Li Xitao; Tao Guanyu; Pan Zhengying; (36 pag.)CN109305944; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com