Iodides-buliding-blocks

624-76-0, name is 2-Iodoethanol, belongs to iodides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. 624-76-0

Preparation of tert-butyl(2-iodoethoxy)dimethylsilane After 2-iodoethanol (1.72 g, 10 mmol) was dissolved in dimethylformamide (8 mL), imidazole (0.817 g, 12 mmol) and tert-butyldimethylsilyl chloride (1.66 g, 11 mmol) were added thereto, and the mixture was stirred for 4 hours at 30 C. to 40 C. Water (50 mL) was added to the reaction solution, and the result was extracted with an ethyl acetate/normal-hexane=1/1 solution (100 mL). The organic layer was washed again with salt water (30 mL*3), dried with anhydrous magnesium sulfate, and then concentrated under reduced pressure to give 2.85 g (90%) of a target compound. This compound was used as it was for the next reaction without purification.

Statistics shows that 624-76-0 is playing an increasingly important role. we look forward to future research findings about 2-Iodoethanol.

Reference:
Patent; KOREA RESEARCH INSTITUTE OF CHEMICAL TECHNOLOGY; SON, Jong Chan; KIM, Bong Jin; KIM, Jae Hak; LEE, Ill Young; YUN, Chang Soo; LEE, Sang Ho; LEE, Chong Kgo; US2014/249162; (2014); A1;,
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

A common compound: 351003-36-6, name is 2-Fluoro-5-iodobenzonitrile, 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. 351003-36-6

To 5-(tributylstannyl)thiazole (1.00 g, 2.7 mmol) in THF (10 mL) was added 2-fluoro-5-iodobenzonitrile (0.791 g, 3.2 mmol). The solution was degassed with N2 and bis(triphenylphosphine)palladium(II) chloride Pd(Ph)2Cl2 (0.187 g, 0.27 mmol) was added. The solution was further degassed for five minutes before heating to 85 C. for 2 h. Upon cooling, the reaction mixture was diluted with saturated NaHCO3 and washed with EA (3¡Á50 mL). The combined organic layers were dried over MgSO4, filtered, and concentrated. The crude product was purified by chromatography (10% EA/Hexanes) to afford 0.450 g (82%) of 2-fluoro-5-(thiazol-5-yl)benzonitrile THZ INT-3 as a tan solid. LCMS-ESI (m/z) calculated for C10H5FN2S: 204.2. found 205.0 [M+H]+, tR=3.00 min.

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, 351003-36-6, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Receptos, Inc.; Boehm, Marcus F.; Martinborough, Esther; Brahmachary, Enugurthi; Moorjani, Manisha; Tamiya, Junko; Huang, Liming; Yeager, Adam Richard; US2015/299179; (2015); A1;,
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

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: 1.00 mmol arylhalide, 1.30 mmol furfural-boronic acid and 0.05 mmolBis(triphenylphosphine)palladium(II) dichloride were treated with 0.30 mLdimethoxyethane, 0.50 mL ethanol and 0.30 mL aqueous 2M sodium carbonate solution.The reaction was heated to 65¡ãC for 1h or until the TLC showed no remaining startingmaterial. The mixture was evaporated and extracted three times with ethyl acetate. Thecombined organic layers were washed with brine, dried over MgSO4, filtered andconcentrated. The crude product was purified by column chromatography usinghexanes/ethyl acetate (9:1).

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:
Article; Krake, Susann H.; Martinez, Pablo David G.; McLaren, Jenna; Ryan, Eileen; Chen, Gong; White, Karen; Charman, Susan A.; Campbell, Simon; Willis, Paul; Dias, Luiz Carlos; European Journal of Medicinal Chemistry; vol. 126; (2017); p. 929 – 936;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

5471-81-8,Some common heterocyclic compound, 5471-81-8, name is Methyl 4-iodo-3-methylbenzoate, molecular formula is C9H9IO2, 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 protective atmosphere of inert gas, Pd(OAc)2 (2.2 mg, 10 mol%), XPhos (19.1 mg, 20 mol%), NBE-CO2K (3.5 mg, were added to a 4.0 mL reaction flask equipped with a magnetic stir bar. 10mol%),Methyl 3-methyl-4-iodobenzoate (0.2 mmol, 1.0 equiv.),Methyl glycidyl ether (0.6 mmol, 3.0 equiv.) and dry N-methylpyrrolidone (1.0 mL). The reaction flask was capped and stirred at room temperature for about 5 minutes, after which the mixture was heated to 80 C and stirred 24hour. After the reaction vessel was cooled to room temperature, it was quenched with water (10 mL), extracted with methyl tert-butyl ether (3¡Á10 mL), dried Na2SO4Dry, filter, and concentrate under vacuum. Purified by column chromatography,The eluent is petroleum ether: ethyl acetate = 10:1 (v/v),34 mg of methyl 7-methyl-2-(methoxymethyl)-2,3-dihydrobenzofuran-5-carboxylate (light yellow oily liquid, yield 72%).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route Methyl 4-iodo-3-methylbenzoate, its application will become more common.

Reference:
Patent; Wuhan University; Zhou Qianghui; Wu Chenggui; Cheng Honggang; (20 pag.)CN108329285; (2018); A;,
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. 612-55-5, name is 2-Iodonaphthalene, This compound has unique chemical properties. The synthetic route is as follows., 612-55-5

General procedure: Aryliodide (0.5 mmol), K4[Fe(CN)6]3H2O(0.15 mmol), K3PO4 (1.5 mmol) and Pd-BNP (5.3 mg, 0.005 mmol, 1.0 mol%)were taken in a oven dried reaction tube equipped with magnetic pellet. DMF(2.0 mL) was added to the reaction tube and the reaction mixture was stirred at120 C temperature. The reaction was monitored by TLC. After consumption ofthe starting material, the reaction mixture was cooled to room temperature.Crude product was extracted with ethyl acetate (3 10 mL). Then the organicphase was dried over Na2SO4 and concentrated in vacuum. The product waspurified by column chromatography using silica gel.

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; Ganapathy, Dhandapani; Kotha, Surya Srinivas; Sekar, Govindasamy; Tetrahedron Letters; vol. 56; 1; (2015); p. 175 – 178;,
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. 76801-93-9, name is 5-Amino-N1,N3-bis(2,3-dihydroxypropyl)-2,4,6-triiodoisophthalamide belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. 76801-93-9

The white powdery product S4 (10 g, 14.2 mmol) obtained in Example 3.Dissolved in 20mL DMAc and acetonitrile mixture (1:1 volume ratio),Cool down to 10 C, control temperature below 30 C,3-chloropropanediol-(1,2) or 2-chloroethanol-1 (10.2 g, 92.3 mmol) was added dropwiseOr 9.55g, 92.3mmol), after the addition is completed, the temperature is raised to 50 C,After stirring for 3 h, it was cooled to 15 C, 20 mL of 10 mol/L NaOH aqueous solution was added dropwise, and the reaction was further stirred at 25 C for 1 h. After the reaction was completed, the pH was adjusted to 4 with dilute hydrochloric acid.Allow to stand at 0 C overnight, filter, filter cake washed with water several times,Drying (drying to constant weight at 85 C),Recrystallization (recrystallization in DMAc mixed with acetonitrile),A white gray or dark gray powder compound is obtained.

The synthetic route of 76801-93-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; China Calculate University; Wu Zhiping; Bai Xueyan; Wu Yuqi; (13 pag.)CN108727376; (2018); A;,
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 3268-21-1 as follows. 3268-21-1

A 200 mL four-neck flask equipped with a stirrer was charged with zinc chloride (7.00 g, 51.4 mmol) and tetrahydrofuran (70 mL) under nitrogen atmosphere, and with stirring, 1,1,1,2-tetrafluoroethane (7.70 g, 75.5 mmol) was blown thereinto at -20 C. Next, a tetrahydrofuran-n-hexane solution of lithium diisopropylamide (1.1 M, 99 mL, 108.5 mmol) was gradually added thereto with the dropping port dipped in the liquid content, and the mixture was stirred at room temperature for 30 minutes. Subsequently, 1,4-diiodo-2,3,5,6-tetramethylbenzene (5.41 g, 14.0 mmol) and tetrakis(triphenylphosphine)palladium (0.65 g, 0.6 mmol) were introduced thereinto and the mixture was stirred at 50 C. for 48 hours. After cooling, an aqueous hydrochloric acid solution was added thereto and the organic layer was washed with 20% saline (50 mL*3 times). The resulting organic layer was dried over anhydrous magnesium sulfate and then the filtrate was concentrated under reduced pressure. The concentrate obtained was purified by silica gel chromatography to give 3.18 g of white solid 1,4-bis(trifluorovinyl)-2,3,5,6-tetramethylbenzene (purity=95.7 wt %, isolated yield=74%). (Results of Analysis) 1H-NMR (Acetone-d6, 400 MHz); 2.18 ppm (d, 12H, Me). 19F-NMR (Acetone-d6, 376 MHz); -158.9 ppm (dd, 2F), -118.3 ppm (ddd, 2F), -104.8 ppm (ddd, 2F). m.p. 91-94 C. GC-MS (m/z):294 (m, 60), 279 (15), 259 (5), 243 (100), 228 (9), 177 (15), 159 (9), 133 (6), 51 (8).

According to the analysis of related databases, 3268-21-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; TOSOH FINECHEM CORPORATION; MIYAUCHI, Hideki; KONDO, Norihisa; NAGASAKI, Noritaka; US2020/17429; (2020); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com