Month: May 2021

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. 624-76-0, name is 2-Iodoethanol, This compound has unique chemical properties. The synthetic route is as follows., Formula: C2H5IO

Add to the reaction bottleThioacetic acid (874 mg, 11.5 mmol),2-iodoethanol (1.72 g, 10 mmol),Dissolved in 15 ml of anhydrous toluene,1,8-diazabicycloundec-7-ene (DBU, 1.75 g, 11.5 mmol) was added dropwise at 0 C.5 ml of toluene solution, plus,The reaction was stirred for 2 hours at room temperature.After TLC detects the reaction,Dilute with a small amount of water,Divide the organic phase,Washed with saturated brine and concentrated.Purified by column chromatography,The product was dried under vacuum to give 576 mg,yield: 48%.

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 624-76-0.

Reference:
Patent; Shenzhen Tajirui Bio-pharmaceutical Co., Ltd.; Wang Yihan; Zhao Jiuyang; (46 pag.)CN109485676; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Some common heterocyclic compound, 181765-86-6, name is Methyl 5-bromo-2-iodobenzoate, molecular formula is C8H6BrIO2, 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. Application In Synthesis of Methyl 5-bromo-2-iodobenzoate

In a 500-mE round-bottom flask reactor, methyl5-bromo-2-iodobenzoate (25.0 g, 73 mmol), 4-dibenzofuran boronic acid (18.7 g, 88 mmol), tetrakis (triphenylphosphine)palladium (1.7 g, 0.15 mmol), and potassium carbonate (20.2 g, 146.7 mmol) were stirred together with toluene (125 mE), tetrahydrofuran (125 mE), and water (50 mE) for 10 hrs at 80 C. Afier completion of the reaction, the reaction mixture was cooled to room temperature and extracted with ethyl acetate. The organic layer thus formed was separated, concentrated in a vacuum, and purified by column chromatography to afford . (75.0 g, 60.1%).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 181765-86-6, its application will become more common.

Reference:
Patent; SFC CO., LTD.; KIM, Hee-Dae; PARK, Seok-Bae; SHIN, Yoona; LEE, Yu-Rim; PARK, Sang-Woo; CHA, Soon-Wook; (81 pag.)US2017/342318; (2017); 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. 355-43-1, name is 1,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-6-iodohexane, This compound has unique chemical properties. The synthetic route is as follows., COA of Formula: C6F13I

In a 1000 mL four-necked flask equipped with a mechanical stirrer, a thermometer, and a condenser, 446 g (1 mol) of perfluorohexyl iodide was added.240.2 g (1.0 mol) of sodium sulfide nonahydrate, heated to a temperature of 90 C by stirring;Another 500mL three-neck bottle with a bottom drop device, mechanical agitation, and a condenser tube.3.4 g (moisture content 28%, 0.01 mol) of benzoyl peroxide and 117.8 g (1.05 mol) of n-octene were added in advance at room temperature.Stir well, add a mixture of benzoyl peroxide and n-octene to a 1000 mL four-necked flask at a temperature of 90 C.Control the dropping time for 2.0 hours, control the dropping reaction temperature to 90 C, and add dropwise.The reaction was kept at 90 C for 1.0 hour, the reaction was completed, the temperature was lowered to room temperature, the insoluble matter was removed by filtration, and distilled under reduced pressure.Obtaining 1,1,1,2,2,3,3,4,4,5,5,6,6-tridecafluoro-8-iodotetradecane 548.0 g, content 99.1%, yield 97.3%;Wherein the isomers were 1,1,1,2,2,3,3,4,4,5,5,6,6-tridecafluoro-7-iodomethyltridecane at a content of 0.9%.

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 355-43-1.

Reference:
Patent; Zhejiang Xinhecheng Co., Ltd.; Zhejiang Xinhecheng Pharmaceutical Co., Ltd.; He Jiawei; Qian Hongsheng; Hu Ruijun; Lu Guobin; Zhang Yangyang; Zhang Wenzhi; Zhu Xinjun; Xu Yong; (10 pag.)CN108358747; (2018); 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. 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

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

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,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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

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

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