Continuously updated synthesis method about 1,3-Dichloro-5-iodobenzene

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.

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., Computed Properties of C6H3Cl2I

The 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 °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 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; Ube Industries, Ltd.; EP2332907; (2011); A1;,
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Application of 1-Chloro-3-iodopropane

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-Chloro-3-iodopropane, other downstream synthetic routes, hurry up and to see.

Electric Literature of 6940-76-7, 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. 6940-76-7, name is 1-Chloro-3-iodopropane belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To a solution of 4-bromo- 2,6-dichlorophenol (10.0 g, 41.1 mmol) and l-chloro-3-iodopropane (10.1 g, 49.0 mmol) in DMF (100 mL) was added CS2CO3 (20.2 g, 61.4 mmol) at 20 C. The reaction was stirred at 70 C for 2 hours. TLC showed the reaction was completed. The resulting solution was cooled down and quenched with water (100 mL), extracted with EtOAc (30 mL x 3). The combined organic layers were washed with brine (100 mL), dried over NaiSOr. filtered and concentrated under reduced pressure. The residue was purified by silica-gel column chromatography to give 5-bromo-l,3-dichloro-2-(3-chloropropoxy)benzene (10.0 g, yield: 76.1%) as yellow oil. NMR (400MHz, CHCb-d) d 7.46 (s, 2H), 4.16 (t, .7=5.75 Hz, 2H), 3.85 (t, .7=6.42 Hz, 2H), 2.29 (t, .7=5.93 Hz, 2H).

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-Chloro-3-iodopropane, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; ESSA PHARMA, INC.; THE UNIVERSITY OF BRITISH COLUMBIA; PROVINCIAL HEALTH SERVICES AUTHORITY; ZHOU, Han-Jie; VIRSIK, Peter; ANDERSEN, Raymond John; SADAR, Marianne Dorothy; JIAN, Kunzhong; GOLEC, Daniel Andrew; (220 pag.)WO2019/226991; (2019); A1;,
Iodide – Wikipedia,
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New learning discoveries about 181765-86-6

According to the analysis of related databases, 181765-86-6, the application of this compound in the production field has become more and more popular.

Related Products of 181765-86-6, 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 181765-86-6 as follows.

In FIG. 1A, a chemical reaction, 101, is provided for the formation of methyl 5-bromo-2-trimethylsilylethynyl-benzoate using methyl 5-bromo-2-iodo-benzoate as a starting material. In this reaction, Sonogashira cross-coupling of trimethylsilyl (TMS) acetylene is such that the iodine of methyl 5-bromo-2-iodo-benzoate is replaced with trimethylsilylethyne (TMS) acetylene. For example, in one embodiment, in chemical reaction 101, TMS acetylene is reacts with methyl 5-bromo-2-iodo-benzoate in the presence of a palladium catalyst, for example bis-(triphenylphosphine)-palladium(II) dichloride, denoted Pd(PPh3)2 in FIG. 1A, and a copper catalyst, such as copper iodide, denoted CuI in FIG. 1A, using a deoxygenated solvent or solvent mixture that includes an organic amine, for example 1:1 dimethylformamide (DMF)/diethylamine (Et2NH) solvent solution, at 25 C. Upon completion, the solvent may be removed in vacuo, and the resulting slurry may be purified further by either standard aqueous workup conditions or filtration conditions. The crude product may be purified by recrystallization, column chromatography or by a variety of techniques known to those skilled in the art.

According to the analysis of related databases, 181765-86-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; International Business Machines Corporation; Kobilka, Brandon M.; Kuczynski, Joseph; Porter, Jacob T.; Wertz, Jason T.; (17 pag.)US2017/331044; (2017); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Extended knowledge of 2-Bromo-4-iodo-1-methoxybenzene

The synthetic route of 182056-39-9 has been constantly updated, and we look forward to future research findings.

Electric Literature of 182056-39-9, A common heterocyclic compound, 182056-39-9, name is 2-Bromo-4-iodo-1-methoxybenzene, molecular formula is C7H6BrIO, 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.

At -100 C., 1 mmol of nBuLi (1 eq.) is added to a solution containing 1 mmol of 2-bromo-4-iodo-1-methoxy-benzene dissolved in 15 mL of distilled hexane. After 45 minutes of stirring at this temperature, 0.5 mmol of 3,4,5-trimethoxyacetophenone diluted in 5 ml of distilled toluene is added. This mixture is stirred for hours while letting the temperature rise up gradually and is then slowly hydrolyzed by a saturated NH4Cl solution up to a pH=7-8. After extraction with diethylether (3×20 mL), the collected organic phases are dried on Na2SO4 and concentrated in the rotary evaporator. The raw reaction product is taken up in 10 mL of CH2Cl2 to which a few grains of hydrated APTS is added, and then stirred for 3 hours at room temperature. The solution is washed with a saturated NaCl solution, extracted with CH2Cl24. After drying on Na2SO4 and concentration in the rotary evaporator, an oil is collected which is purified on silica gel. Yield 53%.H1 NMR: delta ppm, CDCl3 300 MHz: 3.65 (s, 3H), 3.78 (s, 6H), 3.85 (s, 3H), 5.30 (s, 1H), 5.70 (s, 1H), 6.50 (s, 2H), 6.80 (d, 1H, J=8.7 Hz), 7.36-7.46 (m, 2H). Mass spectroscopy (ESI) [M+Na]+=403. Elemental analysis: (MM=378.05) Calculated C, 57.01; H, 5.05. Found C, 56.78; H, 4.90.

The synthetic route of 182056-39-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; CENTRE NATIONAL DE LA RECHERCHE SCIENTIFIQUE (CNRS); US2010/129471; (2010); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 627-32-7

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, 3-Iodo-1-propanol, other downstream synthetic routes, hurry up and to see.

Reference of 627-32-7, 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. 627-32-7, name is 3-Iodo-1-propanol belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

25 g (0.134 mol) of 3-iodopropanol, 26 g (0.202 mol) of diisopropylethylamine and 150 mL of 1,2-dichloroethane Add 250mL three-necked flask, cooled to 0 .Under stirring, a solution of 56.9 g (0.202 mol) of trifluoromethanesulfonic anhydride was slowly added dropwise at a temperature of 0 C. After the addition was completed, the temperature was naturally raised to room temperature and the reaction was allowed to proceed overnight.After the reaction was completed, 30 mL dilute hydrochloric acid (0.1 mol / L) was added to the reaction solution, and the mixture was separated by stirring to extract the organic phase. The organic phase was washed with 0.1 mol / L sodium carbonate aqueous solution and saturated sodium chloride aqueous solution, The organic phase was dried over anhydrous sodium sulfate and concentrated to give 33 g of 3-iodopropyltrifluoromethanesulfonate in a yield of 77%.

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, 3-Iodo-1-propanol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Hebei Sangdiya Pharmaceutical Co., Ltd.; Liu Haitao; Yang Xin; Han Yuchao; Ru Qingke; He Lei; Xia Junyi; Lang Hengyuan; (8 pag.)CN106588731; (2017); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Some tips on C7H4BrIO

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, 5-Bromo-2-iodobenzaldehyde, other downstream synthetic routes, hurry up and to see.

Electric Literature of 689291-89-2, 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. 689291-89-2, name is 5-Bromo-2-iodobenzaldehyde belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Step 2: (5-Bromo-2-iodo-benzyl)-ethyl-amine To 5-bromo-2-iodo-benzaldehyde (5.0 g, 16.1 mmol) in MeOH (20 mL) was added ethylamine (2M in MeOH; 16 mL, 24.0 mmol), followed by acetic acid (1.0 mL, 17.8 mmol), and the mixture was stirred at room temperature for 30 minutes. Sodium cyanoborohydride (2.0 g, 31.8 mmol) was then added over 5 minutes, and the reaction was stirred at room temperature over the weekend. The mixture was concentrated and partitioned between EtOAc and saturated aqueous NaHCO3. The aqueous layer was extracted with EtOAc, and the combined organic layers were dried over MgSO4, filtered, and concentrated. The residue was purified by silica gel chromatography (0-5% MeOH in CH2Cl2) to give the title compound.

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, 5-Bromo-2-iodobenzaldehyde, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; AMIRA PHARMACEUTICALS, INC.; US2009/197959; (2009); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Sources of common compounds: Methyl 3-iodobenzoate

According to the analysis of related databases, 618-91-7, the application of this compound in the production field has become more and more popular.

Synthetic Route of 618-91-7, 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 618-91-7 as follows.

General procedure: A mixture of substituted iodobenzene (2 mmol), (5-formylfuran-2-yl)boronic acid (420 mg, 3mmol, 1.5 equiv), Pd(Ph3P)2Cl2 (0.1 mmol, 0.05 equiv, 70 mg) and potassium carbonate (6 mmol,3 equiv, 828 mg) in dioxone/H2O (6 mL/2 mL) was stirred at 100 C under argon atmosphereuntil the starting material was consumed (typically 20 h). The reaction mixture was then diluted with 25 mL of saturated brine. The mixture was then extracted with EtOAc (25 mL × 2), and the organic layers were combined, dried over Na2SO4. The concentrated crude product was purifie dby column chromatography to afford c2a-e. The second step is the same as procedure A.

According to the analysis of related databases, 618-91-7, the application of this compound in the production field has become more and more popular.

Reference:
Article; Liang, Dongdong; Robinson, Elizabeth; Hom, Kellie; Yu, Wenbo; Nguyen, Nam; Li, Yue; Zong, Qianshou; Wilks, Angela; Xue, Fengtian; Bioorganic and Medicinal Chemistry Letters; vol. 28; 6; (2018); p. 1024 – 1029;,
Iodide – Wikipedia,
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New learning discoveries about C7H4IN

Statistics shows that 3-Iodobenzonitrile is playing an increasingly important role. we look forward to future research findings about 69113-59-3.

Electric Literature of 69113-59-3, These common heterocyclic compound, 69113-59-3, name is 3-Iodobenzonitrile, 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.

General procedure: A solution of Ar3In or (RC?C)3In (0.37mmol, ca. 0.18M in dry THF) was added to a mixture of MCM-41-N,N-Pd(0) (25mg, 1mol%) and aryl iodide (1mmol) in dry THF (2mL) under Ar. The resulting mixture was refluxed under Ar until the starting material had been consumed (TLC). After being cooled to room temperature, the mixture was diluted with Et2O (30mL) and filtered. The palladium catalyst was washed with DMF (2×5mL), Et2O (2×5mL) and reused in the next run. The filtrate was washed with sat. aq NaHCO3 (5mL), water (3×10mL) and dried over MgSO4, filtered, and concentrated under vacuum. The residue was purified by flash chromatography on silica gel to give the desired cross-coupling product.

Statistics shows that 3-Iodobenzonitrile is playing an increasingly important role. we look forward to future research findings about 69113-59-3.

Reference:
Article; Lei, Zhiwei; Liu, Haiyi; Cai, Mingzhong; Journal of Organometallic Chemistry; vol. 852; (2017); p. 54 – 63;,
Iodide – Wikipedia,
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Sources of common compounds: Sodium iodide

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, Sodium iodide, other downstream synthetic routes, hurry up and to see.

Adding a certain compound to certain chemical reactions, such as: 7681-82-5, name is Sodium iodide, 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 7681-82-5, Formula: INa

under a nitrogen atmosphere, and imidazolium salt 2d (20 mg, 0.03 mmol) was added to a 25mL Schlenk tube and dissolved in methylene chloride (2mL). Here silver oxide (7.0 mg, 0.30 mmol) was added, the dark, was stirred at room temperature for 16 hours. The nonbody precipitated afterthe reaction was removed by celite, by distilling a solution to quantitatively obtain silver (Ag) complex compound 7d of interest. Here, methylenechloride (2 mL) was added, PdCl 2 (MeCN) 2 (3.9 mg, 0.015 mmol) and the mixture was stirred at room temperature for 20 hours. After the reactionwas obtained 8d by distilling off the solvent (17.5mg). This was dissolved in methylene chloride (2 mL), sodium iodide (45 mg, 0.3 mmol) and themixture was stirred at room temperature for 20 hours. By distilling off the solvent after the reaction, to obtain a palladium (Pd) complex compound 9dof interest (yield: 19.8mg, 0.012mmol, yield: 80%).

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, Sodium iodide, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; National Institute of Advanced Industrial Science and Technology; Taira, Toshiaki; Imura, Tomohiro; Komura, Nagatoshi; Kitamoto, Dai; (34 pag.)JP2016/98194; (2016); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Continuously updated synthesis method about 127654-70-0

The synthetic route of 127654-70-0 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. 127654-70-0, name is 1-Chloro-3-fluoro-2-iodobenzene, A new synthetic method of this compound is introduced below., Application In Synthesis of 1-Chloro-3-fluoro-2-iodobenzene

2-Chloro-6-fluoro-iodbenzene (10 g, 39 mmol) is dissolved in sulfuric acid (conc., 17 mL) at 0 C. A mixture of nitric acid (conc, 3.2 mL) and sulfuric acid (conc., 3.2 mL) is added at 0 C. and stirring is continued for 2 h at 25 C. The reaction mixture is poured onto ice. The resulting precipitate is collected, dried and used without further purification for the next step.

The synthetic route of 127654-70-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; Stadtmueller, Heinz; US2013/29993; (2013); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com