Category: 3032-81-3

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. 3032-81-3, name is 1,3-Dichloro-5-iodobenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. 3032-81-3

Reference Example 3Synthesis of bis(3,5-dichlorophenyl)sulfideThe compound entitled was synthesized in accordance with the following scheme.Into a 300 ml three-necked glass flask equipped with a thermometer, a reflux condenser and a stirrer, 3,5-dichloroiodobenzene 22.6 g (82.8 mmol) and dimethylformamide 200 ml were added, and argon was passed through the solution for 2 hours and 15 minutes.Then, 3,5-dichlorothiophenol 14.8 g (82.6 mmol), potassium carbonate 22.8 g (165 mmol) and cuprous iodide 1.57 g (8.24 mmol) were added, which were reacted for 3 hours at 95 to 100¡ã C. with stirring.After completion of the reaction, the reaction mixture was cooled down to room temperature and separated with the addition of water and hexane:ethyl acetate (1:1), and the organic layer obtained was dried with anhydrous magnesium sulfate.After filtration, the filtrate was concentrated under reduced pressure, and the obtained concentrate was purified by recrystallization, simple silica-gel column chromatography (eluent; hexane) to obtain bis(3,5-dichlorophenyl)sulfide 25.4 g as white solid (isolation yield; 95percent).

The synthetic route of 3032-81-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; UBE INDUSTRIES, LTD.; US2011/140044; (2011); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding some certain compound to certain chemical reactions, such as: 3032-81-3, name is 1,3-Dichloro-5-iodobenzene, 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 3032-81-3. 3032-81-3

a (3,5-Dichloro-phenylethynyl)-trimethyl-silane The title compound was synthesised from 1,3-dichloro-5-iodo-benzene using the procedure described in Example 18, step (a), in 98percent yield. 1H NMR (CDCl3) delta7.34-7.33 (m, 2H), 7.31-7.29 (m, 1H), 0.24 (s, 9 H).

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 1,3-Dichloro-5-iodobenzene.

Reference:
Patent; 3-Dimensional Pharmaceuticals, Inc.; US2002/169200; (2002); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

The chemical industry reduces the impact on the environment during synthesis 3032-81-3, name is 1,3-Dichloro-5-iodobenzene, I believe this compound will play a more active role in future production and life. 3032-81-3

Example 35 3-(3,5-Dichloro-phenylamino)-4-methoxy-N-phenyl-benzamide Prepared according to the procedure of Example 33 using 3-amino-4-methoxy-N-phenyl-benzamide (2.0 g, 8.3 mmol), 3,5-dichloroiodobenzene (4.5 g, 16.5 mmol), potassium carbonate (2.9 g, 21.0 mmol), and copper(I) iodide (0.5 g, 2.6 mmol) to give a gummy residue which was subjected to chromatography on a column of silica gel in dichloromethane to afford the product (0.3 g); m.p. 207-208¡ã C. after recrystallization from ethanol. Calculated for C20H16Cl2N2O2.0.2C2H6O: C, 61.80; H, 4.37; N, 7.07. Found: C, 61.47; H, 4.04; N, 7.08.

The chemical industry reduces the impact on the environment during synthesis 3032-81-3. I believe this compound will play a more active role in future production and life.

Reference:
Patent; Warner-Lambert Company; US6268387; (2001); B1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

3032-81-3, A common compound: 3032-81-3, name is 1,3-Dichloro-5-iodobenzene, 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.

Compound was obtained following the representative procedure, using 2-phenylimidazo[1,2-a]pyridine 2 (300 mg, 1.5 mmol, 1 equiv), 1,3-dichloro-5-iodobenzene (410 mg, 1.5 mmol, 1 equiv) and heating for 12 h. The crude product was purified by silica gel chromatography using dichloromethane as eluent and trituration with methanol afforded 3-(3,5-dichlorophenyl)-2-phenylimidazo[1,2-a]pyridine 19 as a white powder (347 mg, 68percent yield). Rf = 0.60 (petroleum ether/EtOAc: 7/3); Mp = 210-211 ¡ãC. 1H NMR (400 MHz, DMSO-d6): delta 8.19 (d, 1H, 3J = 6.8 Hz, H5), 7.84 (t, 1H, 4J = 1.6 Hz, He), 7.73 (d, 1H, 3J = 9.2 Hz, H8), 7.65 (d, 2H, 4J = 1.6 Hz, Hd), 7.61 (d, 2H, 3J = 7.2 Hz, Ha), 7.42-7.32 (m, 4H, H7, Hb and Hc), 6.98 (dd, 1H, 3J = 3J’ = 6.8 Hz, H6). 13C NMR (100 MHz, DMSO-d6): delta 144.55 (C), 142.40 (C), 135.27 (2C-Cl), 133.86 (C), 133.16 (C), 129.61 (2Cd), 128.87 (Ce), 128.64 (2Cb), 127.96 (Cc), 127.85 (2Ca), 125.96 (C7), 124.43 (C5), 118.18 (C), 117.05 (C8), 113.16 (C6). IR (KBr) cm-1: 3036 (nuC-Har), 1590, 1560 (nuC=C and nuC=N), 776, 750 (nuC-Cl). MS (ESI) m/z (percent): 339.0 (100) [M + H]+, 341.0 (80) [M + H + 2]+, 343.0 (15) [M + H + 4]+. Anal. Calcd for C19H12Cl2N2: C, 67.27; H, 3.57; N, 8.26. Found: C, 67.50; H, 3.23; N, 7.98.

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, 1,3-Dichloro-5-iodobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Marhadour, Sophie; Marchand, Pascal; Pagniez, Fabrice; Bazin, Marc-Antoine; Picot, Carine; Lozach, Olivier; Ruchaud, Sandrine; Antoine, Maud; Meijer, Laurent; Rachidi, Najma; Le Pape, Patrice; European Journal of Medicinal Chemistry; vol. 58; (2012); p. 543 – 556;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

3032-81-3, A common heterocyclic compound, 3032-81-3, name is 1,3-Dichloro-5-iodobenzene, molecular formula is C6H3Cl2I, 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.

3,5-dichloro-iodo-benzene (5g, 18 mmol) was stirred at room temperature as a solution in DMF (50 ml.) containing tert butyl acrylate (6.5 mL, 2.5 eq), tetrabutyl ammonium chloride hydrate (5.1 g, 1 eq), potassium acetate (5.4 g, 3 eq) and palladium (II) acetate (~200mg, 30 molpercent) for 5 hours. Reaction mixture was reduced in vacuo, partitioned between water and ethyl acetate. Ethyl acetate fractions were dried over magnesium sulfate, filtered over a small plug of silica gel. Silica gel plug washed with 10 percent Ethyl aceated / n-heptanes to afford 3-(3,5-Dichloro-phenyl)-acrylic acid tert butyl ester after evaporation as a white solid. 1H NMR (400 MHz, DMSO-D6) delta ppm 1.46 (s, 9 H) 6.69 (d, J=16.04 Hz, 1 H) 7.49 (d, J=16.04 Hz, 1 H) 7.59 (t, J=1.89 Hz, 1 H) 7.81 (d, J=1.77 Hz, 2 H).

The synthetic route of 3032-81-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; NOVARTIS AG; WO2009/40410; (2009); 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

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. 3032-81-3, name is 1,3-Dichloro-5-iodobenzene, This compound has unique chemical properties. The synthetic route is as follows., 3032-81-3

A 1000-mL flask equipped with overhead stirrer, condenser and thermometer was charged with l,3-dichloro-5-iodobenzene (99.0 g, 0.36 mol), 1,3-dimethyl 2-(3,5- dichlorophenyl)propanedioate (91.0 g, 0.69 mol), copper(I) iodide (4.0 g, 0.021mol), 2-picolinic acid (5.2 g, 0.042 mol) and cesium carbonate (350 g, 1.07 mol) in 1,4-dioxane (600 mL). The reaction mixture was heated under nitrogen to 90 C for 3 hours. The mixture was then cooled to 30 C, diluted with water (300 mL) and hexane (200 mL), and partitioned. The organic phase was washed with saturated aqueous ammonium chloride solution (200 mL) and concentrated under vacuum to a viscous oil. The resulting material was used directly in the next step.

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; E. I. DU PONT DE NEMOURS AND COMPANY; HOFFMANN, Christian; ZHANG, Wenming; CHEN, Yuzhong; WO2013/192035; (2013); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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. 3032-81-3 name is 1,3-Dichloro-5-iodobenzene, 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. 3032-81-3

Step A Synthesis of 5-hydroxy-5-(3,5-dichlorophenyl)hexanenitrile as an intermediate The Grignard reagent of 3,5-dichlorophenyl iodide was prepared by the reaction of 20.0 grams (0.073 mole) of 3,5-dichlorophenyl iodide and 1.8 grams (0.073 mole) of magnesium turnings in 350 mL of diethyl ether. The reaction mixture was heated at reflux for about three hours and then allowed to cool to ambient temperature. To the Grignard reagent, with stirring, was added dropwise during a 15 minute period a solution of 8.4 mL (0.073 mole) of 5-oxohexanenitrile in 25 mL of diethyl ether. The exothermic reaction caused the reaction mixture temperature to rise to about 30¡ã C. Upon completion of addition, the reaction mixture was stirred for one hour and then was poured into 400 mL of water. The mixture was made acidic with about 80 mL of aqueous 2N hydrochloric acid and extracted with two 200 mL portions of diethyl ether. The combined extracts were dried with magnesium sulfate and filtered. The filtrate was concentrated under reduced pressure to a residue. The residue was subjected to column chroma-tography on silica gel, using 5percent diethyl ether in methylene chloride as the eluant. The product-containing fractions were combined and concentrated under reduced pressure, yielding 8.4 grams of 5-hydroxy-5-(3,5-dichlorophenyl)hexanenitrile. The NMR spectrum was consistent with the proposed structure.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 3032-81-3, and friends who are interested can also refer to it.

Reference:
Patent; FMC Corporation; US5521192; (1996); A;,
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. 3032-81-3, name is 1,3-Dichloro-5-iodobenzene, A new synthetic method of this compound is introduced below., 3032-81-3

1,3-Dichloro-5-iodobenzene (2.73 g, 10 mmol) was added to the reaction flask under an argon atmosphere.3,5-dichlorothiophenol (2.15 g, 12 mmol), cuprous iodide (9.5 mg, 0.5 mmol),Potassium carbonate (6.9 g, 50 mmol) and 50 ml of DMF solvent were stirred and heated to 120 ¡ã C for 12 h.After the reaction was stopped, the solvent was evaporated to dryness and extracted with dichloromethane.Purified by silica gel column chromatography, petroleum ether / dichloromethane mixed solvent (15 / 1, v / v) as a rinse to give a white solid, yield 75percent;

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; South China Xietong Chuangxin Institute; Ying Lei; Hu Liwen; Huang Fei; Cao Yong; (25 pag.)CN109096159; (2018); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com