Category: iodides-buliding-blocks

103962-05-6, 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. 103962-05-6, name is 1-Iodo-4-(trifluoromethoxy)benzene, This compound has unique chemical properties. The synthetic route is as follows.

Preparation of (1S)-N-(2-amino-1-hydroxycarbamoyl-ethyl)-4-(4-trifluoromethoxy- phenylethynyl)-benzamide (5). Resin (3) (120 mg, 0.084 mmol) was swelled in DCM (2 mL) for 1 h and drained. A solution of 4-(trifiuoromethoxy)iodobenzene (4) (96.8 mg, 0.336 mmol) and Et3N (150 muL, 1.10 mmol) in DMF (2.0 mL) was purged with a stream of N2 bubbles for two minutes and added to the resin. After mixing for 5 min, PdCl2(PPh3 )2 (18.0 mg, 0.025 mmol) and CuI (8.0 mg, 0.042 mmol) were added and the mixture shaken for 24 h. The resin was drained, washed with DMF (3×2 mL), DCM (3×2 mL) and cleaved with 10percent TFA/DCM (2.0 mL) for 20 min. The solution was collected and the resin was rinsed with additional 10percent TFA/DCM (1.0 mL). The cleavage fractions were combined, treated with neat TFA (3.0 mL), stirred for 1 h at rt and concentrated by rotary evaporation to give a crude brown residue. Purification by RP-HPLC (C18 column, CH3CN gradient 5-55percent, 0.1percent TFA, UV analysis 300 nm, 28 min) and lyophilization of the collected fractions afforded 9.0 mg (25percent yield) of (5) as a white solid. LRMS (ES+) m/z 408.0 (C19Hi6F3N3O4+H requires 408.11); RP-HPLC (300 nm, 28 min run) 18.0 min.

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; ACHAOGEN, INC.; WO2008/154642; (2008); A2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

These common heterocyclic compound, 19099-54-8, name is 1-Iodo-2-isopropylbenzene, 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. 19099-54-8

0.3 mmol of sodium carbonate and 0.1 mmol of 1,2-bis(4-methoxyphenyl)acetylene,Tetrakis(triphenylphosphine palladium) 0.005 mmol, bis(2-diphenylphosphinophenyl)ether 0.005 mmol,0.2 mmol of [1,1′-biphenyl]-4-ylboronic acid, 0.3 mmol of 2-isopropyliodobenzene, and 1 mL of N,N-dimethylformamide were added to a 15 mL reaction tube.Nitrogen was repeatedly filled 10 times, placed in an oil bath at 120 C, and reacted for 24 hours;Cooled to room temperature, the reaction was diluted with ethyl acetate, washed with water three times, the organic phase dried over anhydrous Na2SO4, filtered, and concentratedPurification by thin layer chromatography to give 30.6mg of the desired product in 60% yield.

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 19099-54-8.

Reference:
Patent; Huaqiao University; Cheng Guolin; Lv Weiwei; (20 pag.)CN109879713; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

The chemical industry reduces the impact on the environment during synthesis 20776-55-0, name is 2-Amino-3-iodobenzoic acid, I believe this compound will play a more active role in future production and life. 20776-55-0

General procedure: A suspention of anthranilic acid A1-A17 (0.001mol), a catalytic amount of triethylamine and 4-isothiocyanato-benzenesulfonamide B17b (0.169g, 0.001mol) in absolute ethanol (25ml) was refluxed for 3. The reaction mixture was filtered while hot, left to cool and the solvent was removed under reduced pressure. The obtained residue was triturated from diethyl ether, filtered and dried under vacuo to obtain titled compound C: 1-17 as a whitish solid.

The chemical industry reduces the impact on the environment during synthesis 20776-55-0. I believe this compound will play a more active role in future production and life.

Reference:
Article; Alafeefy, Ahmed M.; Carta, Fabrizio; Ceruso, Mariangela; Supuran, Claudiu T.; Al-Tamimi, Abdul-Malek S.; Al-Kahtani, Abdulla A.; Bioorganic and medicinal chemistry; vol. 24; 6; (2016); p. 1402 – 1407;,
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, 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

A common compound: 645-00-1, name is 1-Iodo-3-nitrobenzene, belongs to iodides-buliding-blocks compound, it can change the direction of chemical reaction, and react with certain compounds to generate new functional products. A new synthetic method of this compound is introduced below. 645-00-1

General procedure: A round bottom flask was charged with aryl halide (0.5 mmol) and terminal acetylene (0.6 mmol). To the mixture, Pd(OAc)2 (1 mol%), A4 (2 mol%) andK2CO3 (1.5 mmol) were added. The reaction mixture was stirred at roomtemperature in EtOH (4 mL) for the mentioned time. The formation of theproduct was confirmed by monitoring the TLC. The reaction mixture was thenextracted with ethyl acetate (3 10 mL). The extracted layer was dried overNa2SO4 and concentrated in rotary evaporator. The crude product was purifiedby column chromatography over silica gel (Eluent: n-hexane) to obtain thedesired product. The pure products were confirmed by 1H and 13C NMR.

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, 645-00-1, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Das, Sameeran Kumar; Sarmah, Manashi; Bora, Utpal; Tetrahedron Letters; vol. 58; 22; (2017); p. 2094 – 2097;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

135050-44-1, Adding a certain compound to certain chemical reactions, such as: 135050-44-1, name is 3-Chloro-4-iodoaniline, 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 135050-44-1.

The N-(3-chloro-4-iodophenyl)methanesulphonamide used as a starting material was obtained by the reaction of 3-chloro-4-iodoaniline and methanesulphonyl chloride using a similar procedure to that described in the portion of Example 3 which is concerned with the preparation of N-(4-iodophenyl)methansulphonamide.

According to the analysis of related databases, 135050-44-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Imperial Chemical Industries PLC; ICI Pharma; US5236948; (1993); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

A common compound: 135050-44-1, name is 3-Chloro-4-iodoaniline, belongs to iodides-buliding-blocks compound, it can change the direction of chemical reaction, and react with certain compounds to generate new functional products. A new synthetic method of this compound is introduced below. 135050-44-1

5-(Methoxymethylene)-2,2-dimethyl-1,3-dioxane-4,6-dione (21.15 g, 113.62 mmol) was added to 3-chloro-4-iodoaniline (24 g, 94.69 mmol) in EtOH (450 mL). The resulting solution was stirred at 80 C. overnight. The reaction mixture was filtered and the solid collected washed with diethyl ether (400 mL) to afford 5-[(3-chloro-4-iodoanilino)methylidene]-2,2-dimethyl-1,3-dioxane-4,6-dione (37 g, 96%) as a white solid; 1H NMR (400 MHz, DMSO, 30 C.) 1.67 (6H, s), 7.34 (1H, dd), 7.90-7.98 (2H, m), 8.57 (1H, s), 11.20 (1H, s).

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, 135050-44-1, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; ASTRAZENECA AB; Kettle, Jason Grant; Bagal, Sharanjeet; Robb, Graeme Richard; Smith, James Michael; Goldberg, Frederick Woolf; Cassar, Doyle Joseph; Feron, James Lyman; US2019/177338; (2019); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

3032-81-3, 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. 3032-81-3, name is 1,3-Dichloro-5-iodobenzene, A new synthetic method of this compound is introduced below.

General procedure: A suspension of DL-5-methoxypyrrolidin-2-one (3a) or arylaminopyrrolidinones 3b,c (1 equiv), CuI (0.5 equiv), cesium carbonate (2 equiv), and corresponding aryl iodide (1 equiv) in dioxane was placed under a nitrogen atmosphere. The coupling ligand DMEDA (1 equiv) was added dropwise by using a syringe and the mixture was then stirred at 60 ¡ãC for various periods of time (14?88 h). At the end ofthe reaction, the insoluble salts deposited after cooling at r.t. were collected by filtration then washed with dichloromethane. The resulting filtrate was concentrated in vacuo and the residue was partitioned between water and dichloromethane. The organic layer was dried on MgSO4 and evaporated to dryness. The residue was finally purified by chromatography on silica gel column (EtOAc/n-heptane) to afford pure N-arylated compound 40?44.

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:
Article; Baudelet, Davy; Daich, Adam; Rigo, Benoit; Lipka, Emmanuelle; Gautret, Philippe; Homerin, Germain; Claverie, Christelle; Rousseau, Jolanta; Abuhaie, Cristina-Maria; Ghinet, Alina; Synthesis; vol. 48; 14; (2016); p. 2226 – 2244;,
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. 18698-96-9, name is 2-(2-Iodophenyl)acetic acid belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. 18698-96-9

General procedure: Pd(OAc)2 (22.4 mg, 0.10 mmol, 0.1 equiv), Ph3P (57.6 mg, 0.22, 0.22 equiv), and Cs2CO3 (1.63 g, 5 mmol, 5 equiv) were added to a flamedried, sealable vial under argon. Dry, degassed MeCN or DMF (3 mL) was added and the yellow mixture was stirred under argon for approximately 5 min. Aryl iodide (1.00 mmol, 1 equiv), alkyl iodide (10.00 mmol, 10 equiv), and olefin (5.00 mmol, 5 equiv) were added successively to the reaction mixture under argon. The mixture was stirred for 5 min, then solid norbornene (470 mg, 5.00 mmol, 5 equiv) was added. After a final argon purge, the vial was capped and placed in an oil bath that had been preheated to 90 ¡ãC. After 4?10 h, the mixture was cooled to r.t. Reactions performed in MeCN were filtered over a short pad of Celite (eluting with CH2Cl2) and concentrated in vacuo. Reactions performed in DMF were diluted with EtOAc? hexanes (1:1) and washed with brine twice. After drying with MgSO4, the organic layer was filtered and concentrated. The crude products were purified by flash column chromatography (CH2Cl2?hexanes, 1:5, then Et2O?hexanes, 1:100?1:25).

The synthetic route of 18698-96-9 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Qureshi, Zafar; Schlundt, Waldemar; Lautens, Mark; Synthesis; vol. 47; 16; (2015); p. 2446 – 2456;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com