Tag: M.W=500-600

Adding a certain compound to certain chemical reactions, such as: 35453-19-1, name is 5-Amino-2,4,6-triiodoisophthalic acid, 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 35453-19-1, Application In Synthesis of 5-Amino-2,4,6-triiodoisophthalic acid

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 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, 169 MS (ES-) found 593.5 [M-H+], expected 593.7

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, 5-Amino-2,4,6-triiodoisophthalic acid, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Wynn, Duncan; Humphries, Gareth; US2007/264201; (2007); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 35453-19-1, name is 5-Amino-2,4,6-triiodoisophthalic acid, 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 35453-19-1, Safety of 5-Amino-2,4,6-triiodoisophthalic acid

Preparation (A); Synthesis of 5-Amino-2,4,6-triiodo-isophthaloyl dichloride (1); 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 0C. A portion of thionyl chloride (15.2 ml, 0.21 mol) was added dropwise during VA o 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, 169MS (ES-) found 593.5 [M-H+], expected 593.7; Example 8; N,N’,N”-Tris-[(3(N-2,3-dihydroxypropylcarbamoyl)-2,4,6-triiodo-1-hydroxyl acetamide) phenyl] carbamoyl methyl ethane; Starting material and all other materials were commercially available from Aldrich. a) 5-amino-2,4,6-triiodo-isophtaloyl chloride; 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 50C 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 593.7FT-IR (cm”1) 3471, 3372 (NH), 1777 (C=O).

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

Reference:
Patent; GE HEALTHCARE AS; WO2007/94683; (2007); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

These common heterocyclic compound, 2043-53-0, name is 1-Iodo-1H,1H,2H,2H-perfluorodecane, 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. COA of Formula: C10H4F17I

The catalyst was separated from the reaction liquid obtained in Example 5 by filtration, and the unreacted olefin was removed with an evaporator, giving 47.5 g of solid CF3(CF2)7CH2CH2I. A 200-ml SUS autoclave was charged with 47.5 g (0.082 mol) of the obtained solid CF3(CF2)7CH2CH2I, 9.9g (0.090 mol) of potassium acrylate, 25 g of t-butanol (solvent), 0.6 g of hydroquinone (polymerization inhibitor) and 0.01 g of hydroquinone monomethyl ether (polymerization inhibitor), and a reaction was then carried out with stirring at 180C for 6 hours.. As a result, CF3(CF2)7CH2CH2OCOCH=CH2 was obtained at a CF3(CF2)7CH2CH2I conversion rate of 99% and at a selectivity of 88%.. The results of NMR analysis revealed that polymerization of CF3(CF2)7CH2CH2OCOCH=CH2 was not detected.

The synthetic route of 1-Iodo-1H,1H,2H,2H-perfluorodecane has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Daikin Industries, Ltd.; EP1457477; (2004); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 35453-19-1, name is 5-Amino-2,4,6-triiodoisophthalic acid, 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 35453-19-1, Computed Properties of C8H4I3NO4

A. Preparation of 5-Amino-2,4,6-triiodoisophthaloyl Chloride STR25 A slurry of 195.2 g. (0.35 mole) of 5-amino2,4,6-triiodoisophthalic acid in 300 ml. of thionyl chloride was refluxed for 24 hours. During the reflux period the solids dissolved. The solution was cooled to 40 and the solvent evaporated to dryness in vacuum. The gummy residue was dissolved in 250 ml. of tetrahydrofuran and evaporated to dryness. The residue was dissolved in 500 ml. of tetrahydrofuran and washed with a mixture of saturated sodium chloride solution and saturated sodium carbonate. The tetrahydrofuran solution was washed twice with saturated sodium chloride solution and dried over anhydrous calcium chloride. The solution was filtered, diluted with 500 ml. of benzene and evaporated to 450 ml. To this solution 450 ml. of petroleum ether (30-60) was added dropwise with stirring. After standing for 2 hours the solids were isolated and dried to yield 100.5 g. (48%). The material was pure as shown by tlc (silica plate-benzene/acetone 80/20).

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-Amino-2,4,6-triiodoisophthalic acid, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Mallinckrodt, Inc.; US4307072; (1981); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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

EXAMPLE 3 Methylene chloride (112 g) and tetrabutylammonium bromide (3.23 g; 0.1 moles) were charged in this order into a reactor. 5-Amino-2,4,6-triiodoisophthalic acid (55.9 g; 0.1 moles) and, in about 2 hours, thionyl chloride (57.1 g; 0.479 moles) were added to the mixture while keeping the internal temperature below 36 C. and adjusting the addition rate with the gas emission. At the end of the addition. the reaction mixture was kept under reflux (43 C.) for 27 hours. After cooling to about 20 C., water (60 g) was added in small portions. At about half of the addition, the formation of a crystalline precipitate was observed. After filtration, the resultant product was washed with water (5*50 g) and then dried in oven under vacuum at 50 C. for about 21 hours obtaining 5-amino-2,4,6-triiodoisophthalic acid dichloride (49.99 g; 83.8% yield) practically pure by HPLC analysis and by thin layer chromatography.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 5-Amino-2,4,6-triiodoisophthalic acid, its application will become more common.

Reference:
Patent; Bracco International B.V.; US5856570; (1999); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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. COA of Formula: C8H4I3NO4

Synthesis of 5-Amino-2,4,6-triiodo-isophthaloyl dichloride (1)5-Amino-2,4,6-triiodo-isophthalic 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 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, air dried 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 (DMSOd6) 66, 78.4, 148.9, 149.2, 169MS (ES-) found 593.5 [M-H+], expected 593.7

The synthetic route of 35453-19-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; GE HEALTHCARE AS; WO2009/5364; (2009); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

507-63-1, name is Heptadecafluoro-1-iodooctane, belongs to iodides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. COA of Formula: C8F17I

A reaction was conducted in the same manner as in Example 1 except that the perfluoroethyl iodide and the copper catalyst were replaced with 1-iodoperfluorooctane (n-C8F17I) and an organic peroxide, i.e., t-butylperoxyisopropyl monocarbonate (Perbutyl I, manufactured by NOF Corporation), respectively. After cooling the reaction mixture, the reaction product was analyzed by gas chromatography (GC). Table 1 shows the results. TABLE 1 Copper Reaction Ethylene Reaction n-C8F17I catalyst temperature pressure time Conversion g g (wt. % *) C. MPa Min GC % Ex. 2 132 13.4 (10) 80 0.1 105 99.94 Ex. 3 130.8 2.66 (2) 80 0.1 120 99.71 Ex. 4 125.3 2.51 (2) 80 0.55 58 99.89 Ex. 5 155.2 3.11 (2) 120 0.1 56 99.97 Ex. 6 122.5 0.62 (0.5) 120 0.55 40 99.86 Comp. 133.2 0.13 ** 105 0.1-0.2 180 97.7 Ex. 1 * wt. % relative to n-C8F17I ** conducted using t-butylperoxyisopropyl monocarbonate (Perbutyl I) as a catalyst The conversion of each 1-iodoperfluorooctane of Examples 2-6 was more than 99.7%. The selectivity for the resulting ethylene adduct (adduct of one ethylene molecule) was 99.9% or greater in each case.

The synthetic route of 507-63-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Funakoshi, Yoshirou; Miki, Jun; US2005/250966; (2005); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 507-63-1,Some common heterocyclic compound, 507-63-1, name is Heptadecafluoro-1-iodooctane, molecular formula is C8F17I, 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.

Reactions were conducted in the same manner as in Example 1 except that the perfluoroethyl iodide was replaced with 1-iodoperfluorooctane (n-C8F17I). After cooling the reaction mixtures, the reaction products were analyzed by gas chromatography (GC). Table 1 shows the results.; TABLE 1 Copper Reaction Ethylene Reaction n-C8F17I catalyst temperature pressure time Conversion g g (wt. % *) C. MPa Min GC % Ex. 2 132 13.4 (10) 80 0.1 105 99.94 Ex. 3 130.8 2.66 (2) 80 0.1 120 99.71 Ex. 4 125.3 2.51 (2) 80 0.55 58 99.89 Ex. 5 155.2 3.11 (2) 120 0.1 56 99.97 Ex. 6 122.5 0.62 (0.5) 120 0.55 40 99.86 Comp. 133.2 0.13 ** 105 0.1-0.2 180 97.7 Ex. 1 * wt. % relative to n-C8F17I ** conducted using t-butylperoxyisopropyl monocarbonate (Perbutyl I) as a catalyst The conversion of each 1-iodoperfluorooctane of Examples 2-6 was more than 99.7%. The selectivity for the resulting ethylene adduct (adduct of one ethylene molecule) was 99.9% or greater in each case.

The synthetic route of 507-63-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Funakoshi, Yoshirou; Miki, Jun; US2005/250966; (2005); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 35453-19-1, 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. 35453-19-1 name is 5-Amino-2,4,6-triiodoisophthalic acid, 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 1 Preparation of R iopamidol [R-5-(alpha-hydroxypropionylamino)-2,4,6-triiodoisophthalic add di-(1,3 dihydroxyisopropylamide)]. 400g (0.72 Mole) 5-amino-2,4,6-triiodoisophthalic acid should be added to 200 ml thionyl chloride, the mixture boiled and stirred for six hours, and the resulting solution then evaporated. The residue should then be dissolved in anhydrous ethyl acetate, and the solution should again be evaporated to dryness. The solid material should then be dissolved in 4000 ml ethyl acetate, and the solution stirred into an ice-cold solution of 500 g sodium chloride and 200 g sodium bicarbonate in 2.5 liters water. The organic phase should be separated from the aqueous solution, washed with aqueous sodium chloride solution, dried by contact with anhydrous calcium chloride, and evaporated to dryness. The resulting 5-amino-2,4,6-triiodoisophthalyl chloride has a melting point of about 300C when recrystallized from toluene.

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

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.