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., Application In Synthesis of 3-Iodo-4-methylbenzoic acid

INTERMEDIATE 8; [2-methyl-5-(5-methyl-1 ,3,4-oxadiaz -2-yl)phenyl]boronic acid; a) Methyl 3-iodo-4-methylbenzoate; A suspension of 3-iodo-4-methylbenzoic acid (15.00 g, 60.00 mmol) and a 4M solution of hydrochloric acid in dioxane (20.00 mL, 80.0 mmol) in methanol (20 mL) was heated in a sealed tube at 80 C with stirring. After stirring for 3 days, the mixture was cooled and ethyl acetate and saturated aqueous potassium carbonate solution were added. The organic layer was washed with brine, dried (MgS04) and evaporated in vacuo to give the title compound (15.00 g, 95%).LR S (m/z): 277 (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; ALMIRALL, S.A.; AIGUADE BOSCH, Jose; CARRANCO MORUNO, Ines; WO2011/57757; (2011); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

82998-57-0, 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. 82998-57-0 name is 3-Iodo-4-methylbenzoic acid, 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.

3-Iodo-4-methylbenzoic acid (lOg, 38. 16mmol), bis (pinnacolato) diboron (14. 5g, 57. 24mmol), potassium acetate (18. 73g, 190.8mmol) and PdCl2dppf (3.12g, 3. 8mmol) in DMF (200ml) were heated at 80C for 21hrs. The solvent was evaporated from the cooled reaction under vacuum, the residue dissolved in ethyl acetate (300ml) and hydrochloric acid (2N, 300ml) and filtered through celite. The organic phase was separated and the aqueous extracted with ethyl acetate (2 x 300ml). The combined organic extracts were washed with brine (500ml) and dried (magnesium sulphate). The solvent was evaporated under vacuum and the residue absorbed onto silica and applied to a silica flash column. This was eluted with cyclohexane/ethyl acetate (5 : 1). The product fractions were concentrated under vacuum to give 4-methyl-3- (4, 4,5, 5-tetramethyl- [1, 3,2] dioxaborolan-2-yl) benzoic acid. LCMS: retention time 3. 65min. NMR : 8H [2H6]-DMSO 12.83, (1H, b), 8.23, (1H, d), 7.89, (1H, dd), 7.29, (1H, d), 2.51, (3H, s), 1.30, (12H, s).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 3-Iodo-4-methylbenzoic acid, and friends who are interested can also refer to it.

Reference:
Patent; SMITHKLINE BEECHAM CORPORATION; WO2003/93248; (2003); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

82998-57-0, The chemical industry reduces the impact on the environment during synthesis 82998-57-0, name is 3-Iodo-4-methylbenzoic acid, I believe this compound will play a more active role in future production and life.

General procedure: To mixture of compound N-(2-chloro-6-methylphenyl)-2-{[6-[4(1-piperazinyl)-2-methyl -4-pyrimidinyl]amino]-5-thiazolecarboxamide (6) (5.1 mol equivalent), the corresponding carboxylic acid (1:1 mol equivalents), DCC (1:1 molequivalents) and oxyma (1:1 mol equivalents) were charged into 4-necked round bottomed flask along with tetrahydrofuran.The slurry was slowly heated at 63-65 C for 4-5 h. Then cooled slowly to room temperature. The reaction mixture was quenched into demineralized water. The obtained solid was collected by vacuum filtration, washed with demineralized water. Suckdried thoroughly to afford crude product. The above obtainedcrude product was dissolved in hot dimethyl sulfoxide (DMSO) (5 volumes to compound weight) and charcoal treatment was given. The hot solution was slowly diluted with water (6 volumes to DMSO quantity) and cooled slowly to room temperature. The solid was colected by vacuum filtration and washed with 10 mL of demineralized water. Drying of the wet compound to get a white coloured product.

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; Buchappa; Durgaprasad; Suneelkumar; Rani, P. Baby; Babu, K. Ravi; Rao, A. K. S. Bhujanga; Aparna; Asian Journal of Chemistry; vol. 28; 6; (2016); p. 1275 – 1280;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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.

Step 7. N-(1,1-difluoro-2,3-dihydro-3-(4-methylpiperazin-1-yl)-1H-indan-6-yl)-3-iodo-4-methylbenzamide A solution of 3-iodo-4-methylbenzoic acid (79 mg, 0.3 mmol) in SOCl2 (5 mL) was refluxed for 3 h, then evaporated in vacuum to remove residual SOCl2. The residue was dissolved in 5 mL anhydrous THF and added to a solution of triethylamine (37 mg, 0.36 mmol), 1-(1,1-Difluoro-2,3-dihydro-6-amino-1H-indan-3-yl)-4-methylpiperazine (78 mg, 0.3 mmol) and DMAP (2 mg) in 5 mL anhydrous THF in dropwise. The result mixture was stirred at rt for 26 h, and evaporated in vacuum. The residue was purified by chromatography on silica gel (CH2Cl2/CH3OH 97:3) to give 140 mg product as a pale yellow solid (91.5%). LCMS: m/z [M+H]+ 512.1049.

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; Astar Biotech LLC; YU, Chunrong; Huang, Haihong; Zhang, Dongfeng; Li, Peng; US2014/31354; (2014); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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. 82998-57-0

General procedure: 1.10.5. General method K To a suspension of amine derivative (1 eq.), carboxylic acid (1.2 eq.), EDCI.HC1 (1.3 eq.) and HOBt (1.3 eq.) in DMF is added Et3N (2.6 eq.). The reaction mixture is stirred overnight at room temperature. After 48 h, water was added and the mixture is extracted with EtOAc. The organic layers are combined, dried over Na2S04, filtered and evaporated to dryness. The expected intermediate is purified by chromatography of silica gel (elution DCM/ MeOH: 95/5 or 90/10) or preparative LCMS.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 82998-57-0, its application will become more common.

Reference:
Patent; GALAPAGOS NV; SANIERE, Laurent Raymond Maurice; HUCK, Jacques; DYKES, Graeme James; SCHMITT, Benoit Antoine; BLANC, Javier; BUTLER, Anna Sara; BEAUMONT, Stephane Nicolas Alain; BONNATERRE, Florence Marie-Emilie; WO2015/24905; (2015); A1;,
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. 82998-57-0

Add 1 equivalent of potassium t-butoxide to a 25 mL Schlenk reaction tube, add 2 mL of toluene under an argon atmosphere, stir for 30 min, remove the solvent, add 0.02 equivalent of anhydrous copper sulfate and 4.0 equivalent of potassium t-butoxide, and dry in vacuum for 15 minutes. 3 mL of benzonitrile and 1 mL of t-butanol were sequentially added under an argon atmosphere, 2 mmol of 3-iodo-4-methylbenzoic acid was in the reaction tube after adding polytetrafluoroethylene stopper was placed into an oil bath of the reaction 90 C for 24 h. After the reaction is completed, 4 equivalents of formic acid are added, and the solvent is removed by filtration and the residue is purified by column chromatography eluting with petroleum ether / methylene chloride / ethyl acetate (v: v: v = 5:10:1), 6-carboxy-2-phenyl-1H-indole was obtained as a white solid. The yield was 92%.

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; University of Science and Technology of China; Kang Yanbiao; Shan Xianghuan; (12 pag.)CN108863894; (2018); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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. 82998-57-0

i) Production of 3-iodo-N,4-dimethylbenzamide 3-Iodo-4-methylbenzoic acid (9.84 g) was dissolved in THF (50 ml) and thionyl chloride (4 ml) and DMF (0.05 ml) were added. The mixture was heated under reflux for 3 hrs. The reaction mixture was concentrated under reduced pressure to give 3-iodo-4-methylbenzoyl chloride (10.18 g) as a brown powder.

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

Reference:
Patent; Takeda Chemical Industries, Ltd.; Kusaka, Masami; EP1348706; (2003); 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., 82998-57-0

Step 1: 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 70C 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, 1 H), 7.87 (d, 1 H, J = 8.4 Hz), 7.48 (d, 1 H, J = 8.4 Hz), 3.85 (s, 3 H), 3.35 (s, 3H); LC-MS m/z: 277.0 (M+1).

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; Novartis AG; DIERKS, Christine; WARMUTH, Markus; WU, Xu; (20 pag.)EP2162190; (2016); B1;,
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. 82998-57-0, name is 3-Iodo-4-methylbenzoic acid, This compound has unique chemical properties. The synthetic route is as follows., 82998-57-0

3-Iodo-4-methylbenzoic acid (1 mmol) was dissolved in dichloromethane and then oxalyl chloride charged in the vessel at 0 to 50 A catalytic amount of dimethylformamide was chargedin the vessel. The reaction mass temperature was raised to 25-30C and maintained for 16-18 hrs. After completion of the reaction, the reaction mass was distilled to a thick oily mass which was subsequently used for further reaction.

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; APICORE US LLC; KOVI, Ravishanker; KANNAPAN, Jayaraman; THAKOR, Sanjay, F.; NAIK, Ashish; BHARATBHAI, Dhakhada, Chetana; KHICHI, Kuldip, Fatehlal; SHIVNATH, Sahebrao, Patil; (23 pag.)WO2016/201203; (2016); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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. 82998-57-0

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).

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