Tag: M.W=400-500

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

Some common heterocyclic compound, 63262-06-6, name is 1,4-Dibromo-2,5-diiodobenzene, molecular formula is C6H2Br2I2, 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. Computed Properties of C6H2Br2I2

Under the protection of nitrogen, 4.85 g of compound II, 2.50 g of trimethylsilylacetylene, 50 ml of triethylamine, 100 mg of cuprous iodide and 150 mg of dichlorobis(triphenylphosphine)palladium were added.Block the reaction system, stir at room temperature overnight, gas phase detectionReaction process, after the reaction is over,The triethylamine was distilled off under reduced pressure, and the column was eluted with a solvent of n-hexane to afford a crude product.White solid 3.2 g, yield 80%.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 63262-06-6, its application will become more common.

Reference:
Patent; Henan Academy Of Sciences Chemical Institute Co., Ltd.; Zhou Yang; Zhao Yongde; Dai Bencai; Liu Changchun; Wang Lantian; Zhang Yuli; Chai Cuncai; Chen Jieying; (11 pag.)CN108558948; (2018); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 2043-57-4, 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 2043-57-4 as follows.

Specifically, first, 2-(perfluorohexyl)ethyl iodide 21.70g (45.8mmol), 4-mercaptophenol 5.72 g (45.3 mmol), potassium carbonate 7.24 g (52.8 mmol), and put the acetone 50mL in 200mL eggplant flask, 2 days at 65 C, was reflux. After completion of the reaction was transferred to stand by separatory funnel to room temperature. There was separated ethyl acetate and brine after addition of the appropriate amount of water and 1N hydrochloric acid 30mL further added to the aqueous phase and an organic phase. Then, after standing for 30 minutes over anhydrous magnesium sulfate the organic phase, subjected to pleat folding filtered to obtain a filtrate was concentrated with an evaporator solid. The obtained solid was purified by silica gel column chromatography with chloroform to give Compound (A) 18.23g (38.6mmol). The obtained compound (A) is a colorless powder, whose melting point is 65 to 68 C, the yield was 85.2%. Further, an infrared spectrophotometer (manufactured by Shimadzu Corp., trade name “IRPrestige-21”. Similarly below. ), And nuclear magnetic resonance apparatus (Nippon Denshi Co. Ltd., trade name “JMN-LA500”. Similarly below. ) Was thus identified compound (A). The results are shown in the following.

According to the analysis of related databases, 2043-57-4, the application of this compound in the production field has become more and more popular.

Reference:
Patent; YAMAGUCHI UNIVERSITY; OKAMOTO, HIROAKI; MORITA, YUKI; (32 pag.)JP2016/64990; (2016); 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. 355-43-1, name is 1,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-6-iodohexane, A new synthetic method of this compound is introduced below., Formula: C6F13I

In reaction kettleF (CF2) 6-I(1298.5 kg, 2.911 kmol)Was stirred and stirred.Next, Parroyl IPP[Half-life temperature: 40.3 C]AE-3000 so that 20% by massSolution dissolved in (1,1,2,2-tetrafluoroethyl-2,2,2-trifluoroethyl ether)(17.0 kg, 0.017 kmol)And CH2 = CHCH2 (CH2) 5H (336.5 kg, 2.999 kmol)It was dripped at the said reaction kettle.During dripping,The internal temperature was kept at 88-100 C.After completion of drippingKeep the internal temperature at 90-100 C,As a result of analyzing the reaction crude liquid A1 obtained by further stirring for 0.5 hour or more by gas chromatography,It was confirmed that F (CF2) 6CH2CHICH2 (CH2) 5H was contained.From the obtained reaction crude liquid A1,Under reduced pressure (-0.093 kPaG.Less than,Gauge pressure,?G? is added after ?kPa? or ?MPa?. )AE-3000 and excessCH2 = CHCH2 (CH2) 5HIs distilled off,Reaction solution 1a containing F (CF2) 6CH2CHICH2 (CH2) 5H(1622.4 kg) was obtained.

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; AGC glass company; Maeda, Yutaka; Mitsui, Yoshiyuki; Yamane, Shingo; (11 pag.)JP2019/108319; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 19231-06-2, 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. 19231-06-2 name is Bis(4-methoxyphenyl)iodonium bromide, 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.

107.2 g obtained in step (1) was added to the reactor.3,5-diiodo-L-tyrosine copper complex and 1000 ml of water,Then slowly add 1200ml of n-butanol to the inside.After the dropwise addition within 1 h, the reaction was dissolved. Then add 43.8g of diisopropylamineThereafter, 146 g of diphenyl methyl ether iodide bromide was further added. The reaction solution was heated to 90 C, and reacted at 90 C for 2 h, cooled to room temperature, and 280 ml of toluene was added. An additional 200 ml of 10% citric acid solution was added and stirred at room temperature for 2 h, filtered, washed with water and methyl isobutyl ketone. The obtained wet cake was further added with 400 ml of 10% citric acid solution and stirred for 1 h, filtered, and washed with 10% citric acid solution.Drying to give 2-amino-3-(3,5-diiodo-4-(4-methoxyphenoxy)phenyl)propionic acid (compound of formula III) 69.1 g,The yield was 59.3%, and it was used.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, Bis(4-methoxyphenyl)iodonium bromide, and friends who are interested can also refer to it.

Reference:
Patent; Nanjing Tech University; Lu Dingqiang; Chen Li; Wang Xinxian; Ye Hui; (10 pag.)CN109810009; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 19231-06-2, name is Bis(4-methoxyphenyl)iodonium bromide, 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 19231-06-2, Recommanded Product: 19231-06-2

295 parts of the salt represented by the formula (I-17-a)88.25 parts of the compound represented by the formula (I-17-b) and 750 parts of chloroform,And the mixture was stirred at 23 C. for 1 hour.After concentrating the obtained reaction solution, to the obtained residue,1000 parts of tert-butyl methyl ether was added and stirred,By filtration, 328 parts of a salt represented by the formula (I-17-c) was obtained.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, Bis(4-methoxyphenyl)iodonium bromide, and friends who are interested can also refer to it.

Reference:
Patent; SUMITOMO CHEMICAL COMPANY LIMITED; ICHIKAWA, KOJI; FUJITA, SHINGO; ANRYU, YUKAKO; (69 pag.)JP6252292; (2017); B2;,
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. 19231-06-2, name is Bis(4-methoxyphenyl)iodonium bromide, A new synthetic method of this compound is introduced below., category: iodides-buliding-blocks

5.00 parts of the compound represented by the formula (I-2-a) and 25 parts of acetonitrile,After stirring at 23 C. for 30 minutes,2.49 parts of silver oxide was charged,After stirring at 23 C. for 1 hour,It was filtered.9.08 parts of the compound represented by the formula (I-2-c) was charged in the recovered filtrate,Followed by stirring at 23 C. for 12 hours.After filtering the obtained reaction mass,The collected filtrate was concentrated.To the collected residue,100 parts of chloroform and 35 parts of ion exchanged water were added and stirred at 23 C. for 30 minutes,The liquid was separated and the organic layer was taken out.Ion exchanged water (35 parts) was added to the recovered organic layer, and the mixture was stirred at 23 C. for 30 minutes,The liquid was separated and the organic layer was taken out.This washing operation was repeated 5 times.After concentrating the obtained organic layer,To the obtained residue,After adding 50 parts of tert-butyl methyl ether and stirring,By filtration, 11.69 parts of a salt represented by the formula (I-2-d) was obtained.

The synthetic route of 19231-06-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SUMITOMO CHEMICAL COMPANY LIMITED; YOSHIDA, ISAO; ICHIKAWA, KOJI; (76 pag.)JP6244891; (2017); B2;,
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. 19231-06-2, name is Bis(4-methoxyphenyl)iodonium bromide, A new synthetic method of this compound is introduced below., Application In Synthesis of Bis(4-methoxyphenyl)iodonium bromide

Each of the four bis(4-methoxyphenyl)iodonium halides (fluoride, chloride, bromide, iodide) (10 mg) was suspended in C6D6, sealed in a J. Young NMR tube, and heated at 120 C for the times indicated: (fluoride, 2.5 hours; chloride, 5 days; bromide, 5 hours, iodide, 2.5 hours). The reactions were followed by FontWeight=”Bold” FontSize=”10″ H NMR spectroscopy and were deemed completed when a homogeneous solution containing no trace of the diaryliodonium salt starting material was obtained. Representative FontWeight=”Bold” FontSize=”10″ H NMR spectra obtained at the completion of reactions are show in FIG. 1. Different reactivity modes are observed across the series of halides. Thermal decomposition of the diaryliodonium fluoride in d6-benzene gave mostly 4-fluoroanisole and a small amount of 3-fluoroanisole. This side product probably arises from a competing mechanism that involves a benzyne intermediate formed by ortho-proton extraction by the hard base fluoride under these conditions. In contrast, chloride and bromide reacted to provide the corresponding 4-haloanisole in quantitative yield; no 3- halo regioisomers were produced. This can be explained easily; the basicity of chloride and bromide are not high enough to promote benzyne formation by proton abstraction. In contrast to these three reactions, which appear to proceed through two-electron intermediates, the thermal decomposition of bis(4-methoxyphenyl)iodonium iodide produces 4,4′-dimethoxy-biphenyl, h, and an unidentified arene product in addition to the 4-iodoanisole. The biphenyl and h probably result from the formation of free radical intermediates.

The synthetic route of 19231-06-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; NUTECH VENTURES; DIMAGNO, Stephen; HU, Bao; WO2015/147950; (2015); A2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 2043-57-4, name is 1,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-8-iodooctane, 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 2043-57-4, Quality Control of 1,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-8-iodooctane

1-Methylimidazole (4.32 g, 0.52 mol) was partially dissolved in reagent-grade toluene (50 ml) in a large round-bottomed flask and stirred vigorously. 1, 1, 1,2,2,3,3,4,4,5,5, 6, 6-Tridecafluoro-8-iodooctane (26 g, 0.053 mol) was added, and the mixture was heated under reflux at 110 degrees C for 24 hours. The solvent was removed under vacuum giving l-methyl-3- (3, 3, 4, 4, 5, 5, 6, 6, 7, 7, 8, 8, 8 -tridecafluorooctyl) imidazolium iodide (30.5 g) as a waxy solid. Potassium 1,1,2,2- tetrafluoroethanesulfonate (TFES-K, 12 g) was added to reagent grade acetone (100 ml) in a separate round-bottomed flask, and this solution was carefully added to the 1- methyl-3- (3, 3, 4, 4, 5, 5, 6, 6, 7, 7, 8,8,8- tridecafluorooctyl) imidazolium iodide which had been dissolved in acetone (50 ml) . The reaction mixture was heated under reflux for approximately 16 hours. The reaction mixture was then filtered using a large frit glass funnel to remove the white KI precipitate formed, and the filtrate was placed on a rotary evaporator for 4 hours to remove the acetone. The oily liquid was then filtered a second time to yield the product, as shown by proton NMR.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-8-iodooctane, and friends who are interested can also refer to it.

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 2043-57-4 as follows. Recommanded Product: 1,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-8-iodooctane

In the first step, a fluorinated phosphonium salt was synthesized by reacting TPP and 2-perfluorohexyl ethyl iodide accordinto literature procedures [38,39]. Briefly, the fluorinated phosphonium salt was prepared by reacting TPP and fluoroalkyl iodide at 95 C in the absence of solvent. The reaction was continued for 24 h until all of the mixture was solidified. After cooling the resulting solid was washed several times with toluene and ether respectively. Then the white solid was dried at 50 C under vacuum.

According to the analysis of related databases, 2043-57-4, the application of this compound in the production field has become more and more popular.