Category: 2043-53-0

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

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

2043-53-0, name is 1-Iodo-1H,1H,2H,2H-perfluorodecane, 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. Safety of 1-Iodo-1H,1H,2H,2H-perfluorodecane

General procedure: Perfluoroalkylethyl iodide (1.0 mol equiv.) (3-4 mmol) and NaN3 (1.2 mol equiv.) were added to dry DMSO (2 mL) in a 10 mL CEM microwave glass reactor tube, a magnetic stirring bead added and the system sealed. The tube was subjected to stirring and microwave irradiation at 250 W and 65 C for 1 h then immediately cooled to r.t.

The synthetic route of 2043-53-0 has been constantly updated, and we look forward to future research findings.

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. 2043-53-0, name is 1-Iodo-1H,1H,2H,2H-perfluorodecane, This compound has unique chemical properties. The synthetic route is as follows., name: 1-Iodo-1H,1H,2H,2H-perfluorodecane

To a solution of 1H,1H,2H,2H-perfluoro-1-iododecane (8.0 g, 14 mmol) in dry ether (150 ml) at -78 C. under Ar was added t-BuLi (1.7 M in hexane; 35 ml, 21 mmol) dropwise with stirring. The mixture was stirred for 1.5 h at -78 C. and cholodiisopropylrosilane (1.7 ml, 10 mmol) was added to the reaction mixture dropwise. The mixture was stirred for 3 h and then warmed to ambient temperature. The reaction mixture was quenched with saturated NH4Cl aqueous solution and extracted with ether. The extract was dried over anhydrous MgSO4 and concentrated. The dark red liquid residue was passed through short column chromatography on silica gel with hexane to provide diisopropyl-1H,1H,2H,2H-perfluorodecanylsilane in 95% yield (5.3 g, 9.5 mmol) as a colorless liquid.

According to the analysis of related databases, 2043-53-0, the application of this compound in the production field has become more and more popular.

Reference:
Patent; University of Pittsburgh; US6897331; (2005); B2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com