375-80-4 Archives - Iodides-buliding-blocks

Sep-21 News Continuously updated synthesis method about 375-80-4

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

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

New learning discoveries about 375-80-4

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

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

Application of 375-80-4

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.

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.

Continuously updated synthesis method about 375-80-4

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

Brief introduction of 375-80-4

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 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

Introduction of a new synthetic route about 1,6-Diiodoperfluorohexane

The synthetic route of 375-80-4 has been constantly updated, and we look forward to future research findings.

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. HPLC of Formula: C6F12I2

75 mg of a commercial mixture of alpha,omega-diiodoperfluorinated compounds (sold by Apollo Scientific Ltd.) composed of 25% tetrafluoro-1,2-diiodoethane (m=1), 25% octafluoro-1,4-tetraiodobutane (m=2), 25% dodecafluoro-1,6-diiodohexane (m=3) and 25% hexadecafluoro-1,8-diiodooctane (m=4) were solubilized in 1 ml of CHCl3, and separately 20 mg of sequestering agent of formula (CH3)3N+-(CH2)12-N+(CH3)3.2I-, i.e. dodecamethonium iodide, were solubilized in 1 ml of CH3OH.The two solutions were then mixed in a test tube which was then closed. After about 2 hours, the formation of a solid white precipitate was observed, which was filtered, washed twice with CCl4 and dried under vacuum. The results of the performed tests, as reported below, confirmed that this was an adduct of dodecamethonium iodide and dodecafluoro-1,6-diiodohexane.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 50 C. and recovered by recondensation at a temperature of about -198 C.100% pure dodecafluoro-1,6-diiodohexane was then obtained.The following tests were conducted on the crystalline adduct:melting point: 226 C.;IR (cm-1, selective bands): pure dodecamethonium iodide: 3002, 2914, 2851, 1483, 1464, 973, 939, 916, 731; adduct of dodecamethonium iodide and dodecafluoro-1,6-diiodohexane: 3010, 2941, 2867, 1475, 1203, 1141, 1125, 1081, 963, 909, 731. 19F NMR (470.6 MHz, CD3OD, 0.002 M): adduct of dodecamethonium iodide and dodecafluoro-1,6-diiodohexane: Deltadelta(ICF2CF2CF2)2=0.08, Deltadelta(ICF2CF2CF2)2=0.01, Deltadelta(ICF2CF2CF2)2=0.00. An XRD test was performed on the adduct crystal which confirmed the exclusive presence of decamethonium iodide and dodecafluoro-1,6-diiodohexane. In fact, FIG. 3 represents the crystalline structure of the adduct in which the molecules of dodecamethonium iodide (the carbon and nitrogen atoms are light grey coloured and the hydrogen atoms white) alternate with the molecules of dodecafluoro-1,6-diiodohexane (carbon atoms are light grey coloured, hydrogen atoms white and the iodine atoms dark grey) and with the iodide atoms (dark grey coloured). Moreover, it was observed that, at the crystalline state, decamethonium iodide and dodecafluoro-1,6-diiodohexane form alternating parallel layers, since the dodecafluoro-1,6-diiodohexane occupies the cavity defined by the spacer chain between the two nitrogen atoms of the dodecamethonium iodide and the two iodides of the same, due to the iodide-iodine interactions generated.Thus, the following crystallographic measurements are reported: As can be observed, in the adduct crystal, the difference Delta (B-A) between the distance B between the iodide atoms aligned with the molecule of dodecafluoro-1,6-diiodohexane, as shown in FIG. 1, and the distance A between the nitrogen atoms belonging to the same dodecamethonium molecule is equal to 0.688 A and significant of the existence of said interactions I . . . I-.The following tests were performed on the pure dodecafluoro-1,6-diiodohexane:IR (cm-1, selective bands): pure dodecafluoro-1,6-diiodohexane: 1190, 1130, 1039, 887, 763; 19F NMR (470.6 MHz, CD3OD, 0.002 M): pure do decafluoro-1,6-diiodohexane: delta=-63.80 (ICF2CF2)2, -112.02 (ICF2CF2)2. The gas chromatography tests also confirmed that this was only 100% dodecafluoro-1,6-diiodohexane.

The synthetic route of 375-80-4 has been constantly updated, and we look forward to future research findings.

Discovery of 375-80-4

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.

Adding a certain compound to certain chemical reactions, such as: 375-80-4, name is 1,6-Diiodoperfluorohexane, 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 375-80-4, Computed Properties of C6F12I2

General procedure: In a typical procedure (IC2F4)2 (45.40g, 0.1mol) was dissolved in 100mL of acetonitrile and 200mL of water in a 500-mL round-bottomed flask. The solution was made basic with NaHCO3 (30.00g, 0.36mol) and then fresh Na2S2O4 (50.00g 0.28mmol, the ratio is 1:2.8) was slowly added with good stirring at 22C. After 20h, fluorine-19 NMR spectroscopy indicated the reaction was complete by disappearance of the -CF2I signal. The solution (NaSO2C2F4)2 and other byproducts are light yellow.

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:
Article; Mei, Hua; Desmarteau, Darryl D.; Journal of Fluorine Chemistry; vol. 160; (2014); p. 12 – 15;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

A new synthetic route of 375-80-4

Electric Literature 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.

Example 3Purification of dodecafluoro-l,6-diiodohexane (m=3) (via solution)75 mg of a commercial mixture of alpha,omega-diiodoperfluorinated compounds (sold by Apollo Scientific Ltd.) composed of 25% tetrafluoro-l,2-diiodoethane (m=l), 25% octafluoro-1,4- tetraiodobutane (m=2), 25% dodecafluoro-l,6-diiodohexane (m=3) and 25% hexadecafluoro- 1,8-diiodooctane (m=4) were solubilized in 1 ml Of CHCl3, and separately 20 mg of sequestering agent of formula (CH3^N+-(CH2)I2-N+(CH3 )3*2I~, i.e. dodecamethonium iodide, were solubilized in I mI Of CH3OH. The two solutions were then mixed in a test tube which was then closed. After about 2 hours, the formation of a solid white precipitate was observed, which was filtered, washed twice with CCU and dried under vacuum. The results of the performed tests, as reported below, confirmed that this was an adduct of dodecamethonium iodide and dodecafluoro-1,6- diiodohexane.The dodecafluoro-l,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 -198C.100% pure dodecafluoro-l,6-diiodohexane was then obtained. The following tests were conducted on the crystalline adduct:- melting point: 226C;- IR (cm 1, selective bands):? pure dodecamethonium iodide: 3002, 2914, 2851, 1483, 1464, 973, 939, 916, 731;? adduct of dodecamethonium iodide and dodecafluoro-l,6-diiodohexane: 3010, 2941, 2867, 1475, 1203, 1141, 1125, 1081, 963, 909, 731.- 19F NMR (470.6 MHz, CD3OD, 0.002 M):? adduct of dodecamethonium iodide and dodecafluoro-l,6-diiodohexane:deltadelta(lComegaCF2CF2)2 = 0.08, deltadelta(lCF2CF2CF2)2 = 0.01 , deltadelta(lCF2CF2CK)2 = 0.00.An XRD test was performed on the adduct crystal which confirmed the exclusive presence of decamethonium iodide and dodecafluoro-l,6-diiodohexane. In fact, Figure 3 represents the crystalline structure of the adduct in which the molecules of dodecamethonium iodide (the carbon and nitrogen atoms are light grey coloured and the hydrogen atoms white) alternate with the molecules of dodecafluoro-l,6-diiodohexane (carbon atoms are light grey coloured, hydrogen atoms white and the iodine atoms dark grey) and with the iodide atoms (dark grey coloured). Moreover, it was observed that, at the crystalline state, decamethonium iodide and dodecafluoro-l,6-diiodohexane form alternating parallel layers, since the dodecafluoro-1,6- diiodohexane occupies the cavity defined by the spacer chain between the two nitrogen atoms of the dodecamethonium iodide and the two iodides of the same, due to the iodide-iodine interactions generated. Thus, the following crystallographic measurements are reported: As can be observed, in the adduct crystal, the difference delta (B – A) between the distance B between the iodide atoms aligned with the molecule of dodecafluoro-l,6-diiodohexane, as shown in figure 1, and the distance A between the nitrogen atoms belonging to the same dodecamethonium molecule is equal to 0.688 A and significant of the existence of said interactions I- 1~.The following tests were performed on the pure dodecafluoro-l,6-diiodohexane:- IR (cm”1, selective bands):? pure dodecafiuoro-l,6-diiodohexane: 1190, 1130, 1039, 887, 763;- 19F NMR (470.6 MHz, CD3OD, 0.002 M):? pure dodecafiuoro-l,6-diiodohexane: delta = -63.80 (ICF2CF2)2, -112.02 (ICF2CF2)2. The gas chromatography tests also confirmed that this was only 100% dodecafluoro-1,6- diiodohexane.

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