The method of obtaining 1,1,1,2,2-pendaftar-3,3-dichloropropane and 1, 1,2,2,3-pendaftar-1,3-dichloropropene

 

(57) Abstract:

Usage: in the chemistry of galoidovodorodov, in particular pentafluoropropanol - solvents or intermediates in industrial organic synthesis. The inventive product - pentafluoropropane. Reagent 1: tetrafluoroethylene. Reagent 2: diperchlorate. Reagent 3: chloroform. Reaction conditions: catalyst is a Lewis acid at 0 to 120°C. for 2 h.p. f-crystals.

The invention relates to a method of producing pentafluoropropanol, in particular 1,1,1,2,2-pendaftar-3,3 - dichloropropane (hereinafter referred to as R-CA) and 1,1,2,2,3 - pendaftar-1,3-dichloropropene (hereinafter referred to as R-225b), which substitutes industrially important compounds 1,1,2 - trichloro-1,2,2-tryptophan, and less impact on the environment. This invention relates to the removal of chloroform from R-s and/or R-225b.

To date R-s and R-225b receive, for example, a periodic manner, by the reaction of interaction of tetrafluoroethylene (hereinafter referred to as TPV) dichloromethane (hereinafter referred to as R-21) in the presence of a catalyst such as anhydrous aluminum chloride, at 15-100aboutWith in an autoclave or in a glass reactor.

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By the first method, which uses anhydrous aluminum chloride, the selectivity and the yield of the desired product in low yield is only 46-58% . Further, as industrial, this method is uneconomical. Upon completion of the reaction it is necessary to separate the products from the catalyst, collecting them in a cold trap under reduced pressure or treating the catalyst hydrochloric acid and thus separating the products.

In addition, in the reaction products inevitably contains by-products such as chloroform. Because chloroform forms an azeotropic mixture with each of the compounds R-s and R-225b, lost large amounts of R-s and R-225b when removing from a mixture of chloroform, which is carried out by distillation, with the aim of obtaining pure R-s or R-225b.

Although the latter method, which uses a cesium fluoride, and gives excellent selectivity and yield, cesium fluoride is one of the raw materials is very expensive. Further, this method is not suitable for industrial production.

One of the aims of this invention is to provide a new method of obtaining R-s and R-225b with high selectivity and yield.

Another purpose of this invention is the, is it the way to get R-s and R-225b, including the interaction of diperchlorate and TPV with chloroform in the above-mentioned mixture in the presence of a catalyst.

In any of the methods of the present invention the catalyst may be any catalyst exhibiting catalytic activity in the reactions of addition of R-21 and TPV. It is preferable to use as the catalyst Lusulu acid. Examples of catalysts are anhydrous aluminum chloride, anhydrous titanium tetrachloride, anhydrous tin tetrachloride, anhydrous pentachloride antimony, anhydrous zinc chloride, anhydrous ferric chloride, anhydrous aluminum bromide, boron TRIFLUORIDE, etc. can also be used a compound of the formula AlClxFyOz(I) where x, y and z are numbers satisfying the equations:

x + y + 2z = 3,

0 < x < 3

0 y < 3

0z < 3/2, provided that at least one of the numbers y and z is not zero; for example, you can use the chloride-fluoride of aluminium and oxochloride-aluminum fluoride.

Chloride aluminum fluoride, intended for use as catalyst in this invention, can be obtained by the reaction of aluminum chloride with hydrogen fluoride, hydrofluoric kislimu carbon (for example, triptorelin, Tetrafluoroethane, Chlorodifluoromethane, DICHLOROFLUOROMETHANE, trifenilamin, trittenheimer, divorcecelebration, trifluorotrichloroethane and others). They can be used individually or in combinations. You can use them, on the contrary, in combination with chloropetalum. The reaction temperature ranges from 0 to 120aboutC, preferably from 0 to 100aboutC. the Reaction can be carried out in liquid phase or in the steam.

Oxochloride-aluminum fluoride, intended for use as catalyst in this invention, can be obtained by the reaction of activated aluminum oxide with chlorine-, Harper or ftoruglevodorodnye, hydrogen chloride or a mixture of at 100-700aboutC. for Example, put the aluminum oxide in a reaction tube made of stainless steel, Hastelloy or glass, and heated to 300-500aboutWith the current dry nitrogen to thoroughly drying the alumina. Then at a higher temperature, preferably 100-600aboutS, more preferably 200-400aboutC, is passed through the reaction tube of the above-mentioned halogenated hydrocarbons, separately or in a mixture with hydrogen chloride or oxygen. If the processing temperatures below 100aboutWith time obrabotke will be deposited carbon, that reduces the catalytic activity. Reduction of catalytic activity can be avoided by introducing air or oxygen, as disclosed in Japan patent N 27375/1986.

Oxochloride-aluminum fluoride can also be obtained by treating activated alumina with gaseous hydrogen chloride. Activated alumina is heated in a current of dry nitrogen at 400-800aboutTo order it for thorough drying. Then, when the above temperature, preferably at 300-700aboutWith over dried alumina miss hydrogen chloride, pure or diluted with an inert gas (e.g. nitrogen, argon etc), or a chlorofluorocarbon (for example, R-12 (DICHLORODIFLUOROMETHANE), R-21, and so on). The gas is passed usually within 3-10 hours

As aluminum oxide can be used or produced by the industry of the porous aluminum oxide constituting the aluminum oxide forms, and used as a catalyst or for dehydration. Examples are Neobead C, MH, GB and D) all manufactured Mizusaeva Chemical Industries, Ltd., as well as activated alumina kPa, N 1 and N 3) all are made by the company Sumitomo Chemical Company, Ltd.

As not containing hydrogen, chlorine or charterplotter titlename examples are carbon tetrachloride, ferrichloride, fluorocarbons, trittenheimer, 1,1,2-trichloro-1,2,2 - trifluoroethane, 1,1,1-trichloro-2,2,2-trifluoroethane, 1,1,2,2-titrator - 1,2, -dichloroethane, 1,1,1,2-titrator-2,2-dichloroethane, 1,1,2,2 - tetrachloro-1,2-dichloroethane, 1,1,1,2-tetrachloro-2,2-differetn etc. as chlorine or chlorofluorocarbons containing a carbon atom, are hydrocarbons, containing 1-3 carbon atoms, preferably 1 or 2 carbon atoms. Preferred examples are fertiliser, diperchlorate, 1,1,1-Cryptor-2,2-dichloroethane, 1,1,2-Cryptor-1,2 - dichloroethane, 1,1,1-Cryptor-2-chlorate etc.

On the contrary, oxochloride-aluminum fluoride, is used as the catalyst, can be obtained by the reaction of aluminum oxide with an inorganic fluoride, for example with hydrogen fluoride at a temperature of 20-450aboutWith; sulfur fluoride (for example, SF4SF6and others), fluoride Sulfuryl or fluoride sulfonyl at 300-500aboutWith; or with ammonium fluoride (for example, acidic ammonium fluoride, neutral ammonium fluoride, and so on) at a temperature of 20-450aboutWith subsequent processing of the product Harper or chloropetalum chloride or hydrogen.

You can use as a catalyst a mixture of two or more katal is e given the anhydrous aluminium chloride and catalysts of the above formula I.

From the point of view of economy, the most preferred method of carrying out the reaction is continuous, when continuously served raw materials and continuously displays the finished product, although you can also use paliperidone process, when continuously served a certain number of starting materials, then the flow is terminated within a certain time course of the reaction, and then removes the reaction products.

In the proposed according to this invention a method of producing R-s and R-225b possible to conduct the reaction between chloroform, R-22 and TPV in the solvent.

You can use any solvent that is inactive with respect to the catalyst and in which are dissolved chloroform, R-22 and TPV. For example, as a solvent, you can use the chloroform. As solvents can be used tetrafluorodichloroethane, which are by-products of the process of getting hydrochloridetramadol. In addition, as a solvent, you can use traditional solvents, such as chloralkali (e.g., dichloromethane) or chlorphenamine (for example, tetrachlorotetrafluoropropanes).

From the viewpoint of facilitating the reaction, predpochtitel the n net R-225.

When in use as a catalyst is anhydrous aluminum chloride, and the solvent - R-sa, R-225b or mixtures thereof, preparing a suspension of a given quantity of anhydrous aluminum chloride in a solvent, and then loaded into the suspension chloroform, R-22 and TPV, in a predetermined ratio and at a given speed. As reaction, the reaction mixture containing the formed R-s and R-225b, separated from the suspension of anhydrous aluminium chloride and removed from the reactor. The reaction mixture can be separated from the suspension of anhydrous aluminium chloride by conventional methods, for example by filtration in a liquid state, or by distillation in vacuum. The separated reaction mixture is further subjected to purification in the traditional way, for example by distillation, to obtain R-s and R-225b.

The mass ratio between the solvent and the catalyst is at least 2. At ratios less than 2, it is impossible to ensure effective mixing of the reaction system, so that occurs at the initial stage, the trend of decreasing selectivity for R-s and R-225b.

Explain the value of molar ratios between chloroform, R-22 and TPV. The molar ratio of chloroform and R-22 is the flax from 1:2 to 1:10. The molar ratio of chloroform:R-22:TPV is, for example, 1:2:4.

You can first be mixed and then loaded into the reactor chloroform, R-22 and TPV, or you can download them, while mixing. In some cases, the load for some time a certain amount of chloroform and then a mixture of R-22 and TPV.

All the raw materials can be used in liquid or gaseous form.

Pressure is not critical and the reaction can be conducted under reduced pressure. However, from the standpoint of simplicity of construction of the reactor, it is preferable to atmospheric or higher pressure.

The reaction temperature usually ranges from -30 to +120aboutC, preferably from -20 to +60aboutC. If the reaction temperature exceeds 120aboutWith a growing number of by-products and decreases the selectivity for R-s and R-225b. When conducting the reaction at temperatures below -30aboutWith the reaction rate becomes impractical low.

All the raw materials, namely chloroform, R-22 and TPV, are products produced by the industry and marketed. Lysova acid, such as anhydrous aluminum oxide, to provide the S="ptx2">

According to the proposed by the present invention method of removal of chloroform, in the case of use as a catalyst is anhydrous aluminum chloride, preparing a suspension of the catalyst in a mixture of R-sa, R-225b and chloroform, and then load the TPV and R-22 in a certain ratio and at a predetermined temperature. The reaction control gas chromatography, and finishing the reaction, when chloroform is not defined.

The catalyst in suspension is separated from the mixture, to isolate the desired products - R-s and R-225b. To separate the catalyst can according to the above method.

As highlighted in the mixture does not contain chloroform, rectification allows an easy and economical way to get clean R-s and R-225b.

According to the proposed method of removal of chloroform, continuously bubbled TPV and R-22 in a gaseous state through the reaction mixture at atmospheric pressure or load in the autoclave, the reaction mixture, and then load the TPV and R-22 at a pressure equal reaction. The pressure of the reaction is not critical.

The value of the molar ratio of TPV and R-22 is not limited. Use at least one mole of the TPV per mole of R-22. A large excess of TPV NC that possible large losses TPV. From the point of view of economy, the upper limit of the content of the TPV is 3 mol per 1 mol of R-22.

The reaction can be carried out at the above temperature.

The invention will be further clarified by the following examples.

P R I m e R 1. In a 100 ml glass flask equipped with drying tube with silica gel to prevent the ingress of moisture in the reaction system and a tube for gas injection, downloaded chloroform (15 g) and anhydrous aluminium chloride (1 g). For mixed in the flask and the suspension was added TPV and R-22 with a speed of respectively 20 and 10 cm3/min through the tube to enter the gas, during which the flask was cooled externally with ice water so that the reaction temperature was equal to 5-10aboutC. According to the analysis of the reaction mixture by gas chromatography, the reaction amount of chloroform decreased, while the number of R-s and R-225b increased. After 5 h of reaction number reaction mixture was equal to 51 g, the composition corresponded to the next. Chloroform was not detected.

The results of gas chromatography R-sa 53,7% R-225b 31,7% R-224*10,8% Other 3.8% of

(* indicates tetraferriphlogopite).

P R I m m e R 2. Prepared as aeromedical mixture at 0-5aboutC for 2 hours Then boiled away the reaction mixture under reduced pressure and obtained the anhydrous chloride aluminum fluoride.

In the same flask, which was used in example 1 was loaded above the anhydrous chloride aluminum fluoride (2 g) and R-225 (CA:cb=51:49), (40 g). Cooling the flask from the outside with ice water and stirring the mixture with a magnetic stirrer, was loaded into a flask with a speed of 1.33 g/h of liquid chloroform. At the same time mixed with a flow rate of respectively 20 and 10 cm3/min TPV and R-22 and loaded into the flask. After 6 h of reaction number reaction mixture was equal to 68 g, and the composition corresponded to the next. Chloroform was not detected.

The results of gas chromatography R-sa 57,7% R-225b 36,7% R-224*2.3% of the Rest of 3.3% (* indicates tetraferriphlogopite).

P R I m e R 3. In a three-neck flask, 100 ml capacity, equipped with a drying tube with silica gel, loaded a mixture of R-s and R-225 (ratio CA:b=92:8) (40 g) containing 3 mol.% the chloroform. After downloading anhydrous aluminium chloride (3 g), when the flow velocity respectively 10 and 30 cm3/min mixed R-22 and TPV and loaded into the flask, stirring the mixture with a magnetic stirrer and cooling the flask from the outside so that the inside of the flask was supported by the m e R 4. Prepared anhydrous chloride aluminum fluoride in the same manner as in example 2.

In a three-neck flask with a capacity of 500 ml, equipped with a drying tube with silica gel, loaded a mixture of R-s and R-225 (CA:cb=92:8, 400 g) containing 3 mol.% the chloroform. After downloading the above anhydrous aluminium chloride (8 g), mixed R-22 and TPV when the flow velocity, respectively, 40 and 40 cm3/min and loaded into the flask while stirring the mixture with a magnetic stirrer and cooled flask from the outside, to maintain the inside temperature 5aboutC. After 5 h, the concentration of chloroform in the mixture of R-s and R-225b fell to 0.3 mol.%.

P R I m e R 5. In the autoclave of 300 ml of SUS316 downloaded the mixture of R-s and R-225b (CA:cb=52:48; 80 g), which contained a 1.2 mol.% chloroform and anhydrous aluminum chloride (4 g), then, after cooling the autoclave, and removed from it the air under reduced pressure. Then downloaded in a gaseous state R-22 (1.5 g) and TPV (3.3 grams) and the mixture was stirred at 25aboutC for 3 hours Analysis of the liquid in the autoclave by gas chromatography showed that the concentration of chloroform in the mixture of R-s and R-225b fell to 0.1 mol.%.

P R I m e R 6. In a reactor with a capacity of 100 ml, equipped with a cooled ice holodilny aluminium chloride (1 g). The mixture was stirred until the formation of a suspension of anhydrous aluminium chloride in R-sa. Then mixed R-21 and TPV in flow rate and 30 cm3/min, respectively, and loaded into the suspension in the reactor, after which the reaction had begun. After 30 min the temperature of the reaction mixture rose to 40aboutC. In 4 h was continuously applied R-21 and TPV, after which the flow was stopped and filtered chloride of aluminum present in the reactor liquid. The filtrate was analyzed by gas chromatography. Got the following results:

The results of gas chromatography TPV 0,9% R-21 0,1% R-CA,cb 94.5% of CHCl32,0% R-225 2.5 Mass of 33.5 g

In a 100 ml three-neck flask equipped with a drying tube with silica gel, loaded the resulting mixture R-s and R-225 (CA:cb=52:48, 30 g) containing 2 mol.% the chloroform. After downloading anhydrous aluminium chloride (1.5 g) was mixed at flow rates respectively 10 and 10 cm3rpm R-22 and TPV and put the mixture in the flask, stirring its contents with a magnetic stirrer and cooling it from the outside so that the inside of the flask temperature was equal to 5aboutC. After 6 hours, the concentration of chloroform in the mixture of R-225 CA and R-225b fell to 0.1 mol.%.

1. THE METHOD OF OBTAINING 1,1,1,2,2-PENDAFTAR-3,3-D IS 0 - 120oIn the presence of a catalyst of the Lewis acid, wherein the process is conducted in the presence of chloroform, and as perchloromethane use diperchlorate.

2. The method according to p. 1, characterized in that the catalyst is chosen from the group comprising anhydrous aluminum chloride, anhydrous titanium tetrachloride, anhydrous tin tetrachloride, anhydrous pentachloride antimony, anhydrous zinc chloride, anhydrous ferric chloride, anhydrous aluminum bromide, boron TRIFLUORIDE, or a compound of the formula

AlClxFyOz,

where x, y and z are numbers satisfying the equations

x + y + 2z = 3;0 < x < 3;0 and y < 3;0 and z < 3/2,

provided that at least one of the numbers y and z is not zero.

3. The method according to p. 1, characterized in that the reaction is carried out in the absence of additional solvent.

 

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