Tag: M.W=500-600

Electric Literature of 375-80-4, 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. 375-80-4, name is 1,6-Diiodoperfluorohexane belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

55.4 g (0.10 mol) of IC 6 F 12 I obtained in Reference Example 1 and 0.58 g (0.004 mol) of tert-butyl peroxide were added to a reactor having a capacity of 150 ml equipped with a stirrer and a thermometer. Next, VDF was added under reduced pressure until reaching 0.5 MPa, and then heating was carried out at 125 C. for 3 hours. Further, after cooling the reaction solution to 70 C., VDF was added to 0.5 MPa and heated at 125 C. for 3 hours. Further, after cooling the reaction solution to 70 C., VDF was added until it reached 0.5 MPa and heated at 125 C. for 5 hours. A total amount of 12.2 g (0.19 mol) of VDF was fed to the reactor.After cooling and discharge of the residual gas, 300 g of chloroform and 20.2 g (0.20 mol) of triethylamine were added to this product, and the reaction was carried out at 35 C. for 3 hours. 150 g of water and 25 g of a 10% hydrochloric acid aqueous solution were added to the obtained reaction solution, and the liquid separation operation was carried out to obtain an organic layer.Chloroform was distilled off from the organic layer, then distilled,17.8 g (yield 42%) of a 6E-T 2 T fraction (purity 99%) having a boiling point of 76 C. (13.33 kPa) of the following formula (12)3.6 g (yield 7%) of a 6E-1 T fraction (purity 97%) having a boiling point of 63 C. (4.00 kPa) of the following formula (13)9.8 g (yield 20%) of a 6E-T 3 TT fraction (purity 97%) having a boiling point of 74 C. (4.00 kPa) of the following formula (14) and 6 E- 0.8 g (yield 1%) of 2TT fraction (purity 98%) was obtained.The structure of the obtained fraction was confirmed by 1 H-NMR and 19 F-NMR.

The synthetic route of 1,6-Diiodoperfluorohexane has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Tosoh F-Tech Co., Ltd.; Kondo, Norihisa; Kono, Masahiro; (14 pag.)JP2015/81232; (2015); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 375-80-4, 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. 375-80-4, name is 1,6-Diiodoperfluorohexane belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: Two equivalents of stilbazole methacrylate and one equivalent of 1,4-diiodoperfluorocarbons were dissolved in THF at room temperature in a clear borosilicate glass vial. The open vial was placed in a closed cylindrical wide-mouth bottle containing paraffin. The THF was allowed to diffuse at room temperature.

The synthetic route of 1,6-Diiodoperfluorohexane has been constantly updated, and we look forward to future research findings.

Reference:
Article; Kumar, Vijith; Mulder, Dirk J.; Cavallo, Gabriella; Pilati, Tullio; Terraneo, Giancarlo; Resnati, Giuseppe; Schenning, Albertus P.H.J.; Metrangolo, Pierangelo; Journal of Fluorine Chemistry; vol. 198; (2017); p. 54 – 60;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Some common heterocyclic compound, 2043-53-0, name is 1-Iodo-1H,1H,2H,2H-perfluorodecane, molecular formula is C10H4F17I, 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. Quality Control of 1-Iodo-1H,1H,2H,2H-perfluorodecane

(Example 1) A mixture of fluoroalkyl alcohols represented by C2F5(CF2CF2)nCH2CH2OH containing one with n=3 in an amount of 80 mol% and one with n=4 in an amount of 20 mol% was produced by a technique of alcoholification of a mixture of C2F5(CF2CF2)nCH2CH2I. 150g (310mmol) of this fluoroalkyl alcohol mixture, 22.3g (260mmol) of acrylic acid, 50g of toluene, 1.48g (7.78mmol) of p-toluenesulfonic acid and 0.05g of hydroquinone were charged into a 300mL glass reactor equipped with a stirrer and subjected to esterification reaction for 4 hours while distilling off water, to give the reaction mixture having a composition as shown in Table 1. This reaction mixture was charged into a still and subjected to distillation using a rectifier with a theoretical plate number of ten(10) and selecting a pressure inside the rectifier and a still temperature within a range of from 0.3 kPa to 15 kPa and a range of from 100C to 160C respectively depending on compounds to be distilled off, so that toluene, acrylic acid, unreacted alcohols, the fluorine-containing acrylic esters (n=3 and n=4) and substances of high boiling points were distilled off in this order. As a result, the mixture after distillation was given as the distillate which was obtained by cutting toluene, acrylic acid and the unreacted alcohols as an initial distillate and the substances of high boiling points as a final distillate, and thereby contained the fluorine-containing acrylic esters as a main component and had a composition as shown in Table 1. In Table 1, the compositions of the reaction mixture and the mixture after distillation were determined by gas chromatography. Table 1 Component Reaction mixture (excluding toluene) (mol%) Mixture after distillation (mol%)C8F17CH2CH2OH 2.19 NDC10F21CH2CH2OH 0.65 0.03C8F17CH2CH2OCOCH=CH2 74.93 79.81C10F21CH2CH2OCOCH=CH2 18.60 19.50 Other substances of high boiling points 3.63 ND As shown in Table 1, of the impurities contained in the reaction mixture, C8F17CH2CH2OH (n=3) and the substances of high boiling points were able to be removed by the distillation. As a result, the mixture of the fluorine-containing acrylic esters with a high purity was obtained. Specifically, only C10F21CH2CH2OH (n=4) was contained as the impurity in an amount of 0.03 mol%. In this example, an yield of the fluorine-containing acrylic esters was 85 mass%.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2043-53-0, its application will become more common.

Reference:
Patent; DAIKIN INDUSTRIES, LTD.; EP1757577; (2007); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 375-80-4, The chemical industry reduces the impact on the environment during synthesis 375-80-4, name is 1,6-Diiodoperfluorohexane, I believe this compound will play a more active role in future production and life.

11.1 g (0.02 mol) of IC 6 F 12 I obtained in Reference Example 1, 0.16 g (0.001 mol) of ferric chloride FeCl 3 and 15 g of acetonitrile were added to a reactor having a capacity of 150 ml equipped with a stirrer and a thermometer. Next, VDF was added under reduced pressure until reaching 0.5 MPa, and the mixture was heated at 130 C. for 14 hours. A total amount of 3.2 g (0.05 mol) of VDF was fed to the reactor.After cooling and discharging the remaining gas, 6.1 g (0.04 mol) of 1,8-diazabicyclo [5.4.0] -7-undecene was added to this product and the reaction was carried out at 10 C. for 3 hours. After adding 30 g of water and 8 g of a 20% hydrochloric acid aqueous solution to the obtained reaction solution, acetonitrile was distilled off. Further, 40 g of chloroform was added, and an organic layer was obtained by liquid separation operation.Distillation of chloroform from the organic layer was followed by distillation to obtain 1.4 g (yield 16%) of a 6E-T 2 T fraction (purity 99%) having a boiling point of 76 C. (13.33 kPa) of the formula (12)3.4 g (yield 35%) of 6E-1 T fraction (purity 97%) having a boiling point of 63 C. (4.00 kPa) of the formula (13) was obtained.

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, 1,6-Diiodoperfluorohexane, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Tosoh F-Tech Co., Ltd.; Kondo, Norihisa; Kono, Masahiro; (14 pag.)JP2015/81232; (2015); 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 35453-19-1 as follows. HPLC of Formula: C8H4I3NO4

5-Amino-2,4,6-triiodo-isophtalic acid (30 g, 0.054 mol), thionyl chloride (8.2 ml, 0.113 mol) and pyridine (0.2 ml) in 1 ,2 dichloroethane (20 ml) were heated to 70 0C. A portion of thionyl chloride (15.2 ml, 0.21 mol) was added dropwise during VA to 2 hrs, and the mixture was heated to 85 0C for 6 hrs. After cooling the reaction mixture to room temperature, it was poured into 30Og of ice-water. The yellow precipitate that formed was filtered off, sucked dry and then washed with water until washings showed a pH of ca 5. The filter cake was then dried in a vacuum oven at 500C for 3 hrs. A light yellow powder was obtained 31 g (~ quant.) as the desired product. 13C NMR (DMSOcZ6) 66, 78.4, 148.9, 149.2, 169 MS (ES-) found 593.5 [M-H+], expected 593.7

According to the analysis of related databases, 35453-19-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; GE HEALTHCARE AS; WO2007/133090; (2007); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 375-80-4, 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. 375-80-4, name is 1,6-Diiodoperfluorohexane belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

55.4 g (0.10 mol) of IC 6 F 12 I obtained in Reference Example 1 and 0.58 g (0.004 mol) of tert-butyl peroxide were added to a reactor having a capacity of 150 ml equipped with a stirrer and a thermometer. Next, VDF was added under reduced pressure until reaching 0.5 MPa, and then heating was carried out at 125 C. for 3 hours. Further, after cooling the reaction solution to 70 C., VDF was added to 0.5 MPa and heated at 125 C. for 3 hours. Further, after cooling the reaction solution to 70 C., VDF was added until it reached 0.5 MPa and heated at 125 C. for 5 hours. A total amount of 12.2 g (0.19 mol) of VDF was fed to the reactor.After cooling and discharge of the residual gas, 300 g of chloroform and 20.2 g (0.20 mol) of triethylamine were added to this product, and the reaction was carried out at 35 C. for 3 hours. 150 g of water and 25 g of a 10% hydrochloric acid aqueous solution were added to the obtained reaction solution, and the liquid separation operation was carried out to obtain an organic layer.Chloroform was distilled off from the organic layer, then distilled,17.8 g (yield 42%) of a 6E-T 2 T fraction (purity 99%) having a boiling point of 76 C. (13.33 kPa) of the following formula (12)3.6 g (yield 7%) of a 6E-1 T fraction (purity 97%) having a boiling point of 63 C. (4.00 kPa) of the following formula (13)9.8 g (yield 20%) of a 6E-T 3 TT fraction (purity 97%) having a boiling point of 74 C. (4.00 kPa) of the following formula (14) and 6 E- 0.8 g (yield 1%) of 2TT fraction (purity 98%) was obtained.The structure of the obtained fraction was confirmed by 1 H-NMR and 19 F-NMR.

The synthetic route of 1,6-Diiodoperfluorohexane has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Tosoh F-Tech Co., Ltd.; Kondo, Norihisa; Kono, Masahiro; (14 pag.)JP2015/81232; (2015); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 375-80-4, 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. 375-80-4 name is 1,6-Diiodoperfluorohexane, 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.

Example 11Purification of dodecafluoro-l,6-diiodohexane (m=3) (via gas/solid)20 mg of dodecamethonium iodide and 100 mg of dodecafluoro-l,6-diiodohexane of 98% purity (sold by Sigma-Aldrich) were put into two different open test tubes. Both said open test tubes were promptly put into a chamber, which was immediately closed. The dodecafluoro- 1,6-diiodohexane, being very volatile, expand inside the closed chamber, thus contacting the solid dodecamethonium iodide. Once the dodecafluoro- 1,6-diiodohexane was left to spread for 6 hours at room temperature, the formation of a yellow solid was observed which was extracted from the chamber, washed with CCU and dried under vacuum. On the solid thus obtained, 1H and 19F NMR tests were carried out in the presence of (CFaCH2O)2 as internal standard; such tests confirmed the formation of an adduct composed of two compounds in 1 :1 ratio. An XRD test was performed on the adduct crystal which confirmed the exclusive presence of dodecamethonium iodide and dodecafluoro- 1,6-diiodohexane and allowed to observe the same crystalline phase of the adduct obtained in Example 3.The dodecafluoro- 1,6-diiodohexane was then separated from the sequestering agent by sublimation of the crystalline adduct under vacuum at a temperature of about 500C and recovered by recondensation at a temperature of about -1980C.It was then possible to further purify the dodecafluoro- 1,6-diiodohexane available on the market with a 98% purity to dodecafluoro- 1,6-diiodohexane with a 100% purity, through a process of the invention from gas phase on solid phase, thus obtaining the same optimal results of the process of the invention from liquid phase.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1,6-Diiodoperfluorohexane, and friends who are interested can also refer to it.

Reference:
Patent; Politecnico di Milano; WO2009/7302; (2009); A2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 35453-19-1, A common heterocyclic compound, 35453-19-1, name is 5-Amino-2,4,6-triiodoisophthalic acid, molecular formula is C8H4I3NO4, 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.

5-Amino-2,4,6-triiodo-isophtalic acid (30 g, 0.054 mol) (commercially available from Aldrich), thionyl chloride (8.2 ml, 0.113 mol) and pyridine (0.2 ml) in 1,2 dichloroethane (20 ml) were heated to 70 C. A portion of thionyl chloride (15.2 ml, 0.21 mol) was added dropwise during 1½ to 2 hrs, and the mixture was heated to 85 C. for 6 hrs. After cooling the reaction mixture to room temperature, it was poured into 300 g of ice-water. The yellow precipitate that formed was filtered off, sucked dry and then washed with water until washings showed a pH of ca 5. The filter cake was then dried in a vacuum oven at 50 C. for 3 hrs. A light yellow powder was obtained 31 g (quant.) as the desired product.13C NMR (DMSOd6) 66, 78.4, 148.9, 149.2, 169MS (ES-) found 593.5 [M+H+], expected 593.7

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; GE HEALTHCARE AS; US2008/260651; (2008); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 35453-19-1, 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. 35453-19-1, name is 5-Amino-2,4,6-triiodoisophthalic acid belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

The product (S2) obtained in the step 1) of Example 2, 3,5-dicarboxy(2,4,6)triiodoaniline (10 g, 0.018 mol) was dissolved in 40 mL of ethyl acetate.60 mL of SOCl2 (8.6 g, 0.072 mol) was slowly added dropwise at 70 C.(The purpose of the dropping control temperature does not exceed 10 C), after the addition is completed, the temperature is raised to 80 C,The reaction was refluxed for 20 h, and about half of the solvent was distilled off.Allow to stand for 2 hours, filter, and dry (85 C drying to moisture content ? 1.5%),A brownish brown powdery compound (S3) was obtained.

The synthetic route of 5-Amino-2,4,6-triiodoisophthalic acid 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

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. 35453-19-1, name is 5-Amino-2,4,6-triiodoisophthalic acid, This compound has unique chemical properties. The synthetic route is as follows., Application In Synthesis of 5-Amino-2,4,6-triiodoisophthalic acid

In step 1, the product formed after the reaction of the compound A and the iodine chloride is compound B, 100 g of the compound B and 150 g of phosphorus pentachloride are mixed in a vessel, the reaction temperature is controlled at about 30 degrees Celsius, and the reaction time is controlled at 40 minutes. After the reaction is completed, a small amount of a chlorinating agent needs to be added to the reaction vessel. The chlorinating agent may be hydrochloric acid, and about 20 g of hydrochloric acid is added. After reacting for 10 minutes, it is rinsed with water, and then filtered to obtain a compound C.

According to the analysis of related databases, 35453-19-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Hubei Tianshu Pharmaceutical Co., Ltd.; Liu Yunlong; (12 pag.)CN109293526; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com