The method of obtaining alkoxyacetic acids or their salts

 

(57) Abstract:

The inventive product is alkoxyalkane acid or their salts, f - crystals: RO(CH2CH2O)nR - octylphenyl, nonylphenyl, dodecylphenyl, primary or secondary alkyl, C10-C20n-3 - 20. Acid number 51 - 91. Reagent 1: connection of General f - crystals: RO(CH2CH2O)n, R, n is specified. Reagent 2: oxygen-containing gas. Reaction conditions: 80 - 130C and 0 to 10 ATM at the stationary layer of the catalyst is Pd/c, when the supply of reagents in the form of foam. table 2.

The invention relates to an improved method for producing alkoxyacetic acids (AUC) and their salts, which are used as surface-active substances [1] .

A method of obtaining alkoxyacetic acids and their salts by oxidation with oxygen or oxygen-containing gas polyoxyethyleneglycol esters in aqueous buffer solution at 80aboutWith in a tubular bubble column in the presence of a catalyst to 6.5% Pd on charcoal and additives lower oxyalkylated phenol [2] .

The main disadvantages of this method are the periodicity of the process, the use of a substantial excess of the base and additive compounds, which is x salts by oxidation with oxygen polyoxyethyleneglycol esters (PE) in aqueous-alkaline solution at 50-95aboutAnd 0-3 ATI catalyst 1-10 wt. % palladium on coal in an autoclave, where the source reagents are served after intensive mixing. ,

The main disadvantages of this method are the difficulties associated with separating fine catalyst from the viscous reaction mass, as well as the relatively low conversion of the original polyoxyethyleneglycol ether.

Technical solution to the problem is to simplify the process and increase the degree of conversion.

This task is solved by the oxidation of oxygen-containing gas compounds of General formula

RO(CH2CH2O)nH, where R is octylphenyl, nonylphenyl, dodecylphenyl, primary or secondary alkyl, C10- C20;

n = 3-20, in aqueous-alkaline medium at 80-130aboutWith and 0-10 MPa in the presence of a catalyst of palladium on coal, while the oxidation of lead in the continuous mode when the supply of reagents in the form of foam on a stationary catalyst bed.

Distinctive features of the process is that the oxidation of lead in continuous mode at 80-130aboutWith and 0-10 MPa when applying reagents in the form of foam on the fixed catalyst bed, which allows you to simplify the process and increase the conversion rate.

The process proceeds in the mode of displacement, i.e., when the continuous supply of reactants to the reactor and the continuous removal of products from the reactor, thereby creating a continuous mode.

P R I m e R 1. The process is carried out in a tubular reactor with a volume of 0.5 l, filled heterogeneous catalyst 2% palladium on charcoal brand AG-3, and is equipped with a thermostatic jacket to maintain the desired temperature. As a source of reagent use sintana DS-20, (TC 6-06-C5-84), representing polyoxyethyleneglycol esters of primary alcohols fraction10-C18with the average number of hydroxyethyl groups, equal to 20 (R = C10- C18, n = 20), a hydroxyl number (MS) equal to 52, the average molecular mass (MM), equal to 1080, the General formula: RO(CH2CH2O)20H. the oxidation Process is carried out in nepreryvnolitoj from the reactor.

In the upper part of the reactor continuously in the form of foam serves a mixture of aqueous-alkaline solution cintanya DS-20 composition, wt. % : sintana 20,0; NaOH 0,76; water - the rest, with a rate of 0.36 kg/h, and oxygen-containing gas composition, vol. % : oxygen 97; nitrogen - rest, with a speed of 1.9 nl/h, which is previously obtained from the supply source flows an aqueous-alkaline solution cintanya DS-20 and oxygen in the ejector. The temperature in the reactor 90aboutC. the Pressure is atmospheric. Gas-liquid mixture emerging from the reactor is sent to a separator gas-liquid selected liquid phase containing the catalyst, which is analyzed by the method of non-aqueous titration [4] the content of sodium salt alkoxyalkyl acid. 3 hours of continuous work submitted in response 216 g (0.2 mol) of cintanya received 211 g (0,189 mol) of sodium salt alkoxyalkyl acid of General formula: RO(CH2CH2O)19OCH2COONa. The degree of conversion of cintanya amounted to 94.5% . To obtain alkoxyalkyl acid oxidat acidified with concentrated hydrochloric acid and extracted with chloroform. From the obtained chloroformate extract is distilled chloroform and obtain 198 g (0,181 mol) alkoxyalkyl acid with an acid number of 51. Output auctions per taken si is any DC-10 (THE 6-14-577-77), representing polyoxide - longicollis esters of primary alcohols fraction10-C18with the average number of hydroxyethyl groups, equal to 9 (R = C10- C18n = = 9, MS= 94, MM= 596).

As the catalyst used 4% Pd on charcoal brand ARB.

In the upper part of the reactor continuously in the form of foam serves a mixture of aqueous-alkaline solution cintanya DC-10 composition, wt. % : sintana 10,8; NaOH 0,73; water - the rest, with a rate of 0.36 kg/h and oxygen-containing gas composition, vol. % : oxygen 93; nitrogen - rest, with a speed of 2.0 nl/h Temperature in the reactor 90aboutC. the Pressure is atmospheric. The reaction filed 111,6 g (0,196 mol) sentenela received 117,5 g (0,186 mol) of sodium salt alkoxyalkyl acid. The conversion rate was 94.9% . After acidification and extraction get to 108.8 g (0,178 mol) alkoxyalkyl acid with an acid number 92. The output APK - 90,8 mol. % .

P R I m e R 3. The process is carried out in a tubular reactor with a volume of 4 liters, filled with a heterogeneous catalyst (1 wt. % Pd on charcoal brand AR-3, and is equipped with a thermostatic jacket to maintain the desired temperature. As the source reagent is used neonol AF-10 (TU 38103625-87), representing policies, MM = 660).

In the upper part of the reactor continuously in the form of foam serves a mixture of aqueous-alkaline solution of neonols AF-10 composition, wt. % : neonol 10,0; NaOH 0,61; water - the rest, with the speed of 2.15 kg/HR and air at a rate of 150 nl/h Temperature in the reactor 122aboutC. the Pressure of 6.0 MPa. For 8 hours of continuous operation filed 1,72 kg (2,61 mol) of neonols received 1,77 kg (2.54 mol) of sodium salt alkoxyalkyl acid. The degree of conversion of neonols - 97,3% . After acidification and extraction of the gain of 1.66 kg (2,47 mol) alkoxyalkyl acid with an acid number 83. The output APK - 94,6 mol. % .

P R I m e R 4-6. The process is carried out analogously to example 3, giving the oxidation polyoxyethyleneglycol esters of primary alcohols other factions. Conditions and results of oxidation are presented in table. 1 and 2.

P R I m e R s 7-13. The process is carried out analogously to example 1, applying the oxidation polyoxyethyleneglycol ethers of alkyl phenols and alcohols. Conditions and results of oxidation are presented in table. 1 and 2.

The process in this way allows you to avoid phase separation of the catalyst and to increase the degree of conversion polyoxyethyleneglycol esters with 81-94 to 94,5-100% . (56) 1. The Schoenfeld N. Surfactants based on hydroxy who 614, CL 07 With 51/235, publ. 1981.

4. Sigma S. and Hanna, Quantitative analysis of functional groups. M. : Chemistry, 1983, S. 136.

The METHOD of OBTAINING ALKOXYACETIC ACIDS OR THEIR SALTS by oxidation of oxygen-containing gas compounds of General formula

RO (CH2CH2O)nH,

where R is octylphenyl, nonylphenyl, dodecylphenyl, primary or secondary alkyl, C10- C20;

n = 3 - 20,

in aqueous-alkaline medium at elevated temperature in the presence of a catalyst of palladium on charcoal, characterized in that oxylene are in continuous mode at 80 - 130oC and 0 to 10 MPa when applying reagents in the form of foam on a stationary catalyst bed.

 

Same patents:

FIELD: organic chemistry, chemical technology.

SUBSTANCE: invention relates to the improved method for preparing 2-keto-L-gulonic acid. This compound is an intermediate substance in synthesis of vitamin C. Method involves oxidation of L-sorbose in the presence of platinum-containing polymeric catalyst applied on Al2O3 in medium with the equimolar content of NaHCO3 under atmosphere pressure, at the rate stirring 870-1 000 rev/min and bubbling pure oxygen as an oxidizing agent. Reaction is carried out in medium water : ethyl alcohol 7-10 vol. %, in the concentration of L-sorbose 0.29-0.6 mole/l, on spherical microparticles of catalyst in the amount 20-40 g/l with ultra-thin layer of polydiallyldimethylammonium chloride as cationic polyelectrolyte with platinum nanoparticles formed on it. The content of platinum in catalyst is 1-2%. The feeding rate of oxidizing agent is 400-450 ml/min. The end product is obtained with high yield 97-99%.

EFFECT: improved preparing method, enhanced yield of product.

7 cl, 1 tbl, 1 sch, 7 ex

FIELD: organic chemistry, chemical technology.

SUBSTANCE: invention relates to a method for preparing 2-ethylhexanoic acid. Method involves catalytic hydrogenation of fraction isolating from the manufacturing waste in the presence of hydrogen by rectification method followed by oxidation of prepared hydrogenation product with air oxygen at temperature 30-80°C and under pressure 0.1-1.0 MPa. Vat residue from rectification of butyl alcohols in oxo-synthesis is used as raw for the process. Fraction with the total content of unsaturated and saturated C8-alcohols 65-95 wt.-% is isolated from vat residue by rectification and in residual pressure on column top 100-300 mm of mercury column. This fraction is subjected for hydrogenation in vapor phase under atmosphere pressure, temperature 220-270°C, volume rate of raw feeding 0.5 h-1, volume ratio raw : hydrogen = 1:1 on copper-containing catalyst and the following isolation 2-ethylhexanal from catalyzate by rectification on two columns working at residual pressure on top of the first column 60-100 mm of mercury column and on top of the second column 20-80 mm of mercury column, and 2-ethylhexanal is oxidized with air oxygen. The end 2-ethylhexanoic acid is isolated from the prepared oxidized product by rectification on two columns working at residual pressure on top of column 20-70 and 10-60 mm of mercury column, respectively. Method provides enhancing the yield of 2-ethylhexanoic acid.

EFFECT: improved method for preparing.

2 cl, 16 ex

FIELD: organic synthesis.

SUBSTANCE: synthesis involves oxidation of substrate with chlorine dioxide in organic solvent at 40-50°C, said selected from myrtenal or myrtenol and said organic solvent from acetone, benzene, and alcohol at molar ratio of myrtenal or myrtenol to chlorine dioxide 1:(0.5-3.5). Thus formed myrtenic acid is isolated in the form of its water-soluble salt and, when alcohol is used as solvent, in the form of ester.

EFFECT: increased yield of product to 66%, reduced expenses, and shortened reaction time.

3 cl, 1 tbl, 2 ex

FIELD: industrial organic synthesis.

SUBSTANCE: invention provides improved process for production of isobutyric acid suitable for use in production of higher carboxylic acid esters and drying oils. Process comprises oxidation of isobutyric aldehyde with air oxygen on heating in column-type reactor filled with zeolite of types CaX, CaA, NaX, or NaA with packing diameter-to-packing width ratio 1:(7.2-8), at volumetric air supply velocity 684.0-874.0 h-1, butyric acid-to oxygen molar ratio 1:(0.7-1.0), and temperature 62-66°C.

EFFECT: increased yield of desired product and intensified process.

3 tbl, 4 ex

FIELD: heating.

SUBSTANCE: invention concerns improved method of catalytic oxidation in vapour phase which supplies effective removing of reactionary heat, excludes hot spot formation, and supplies effective receipt of base product. Method of catalytic oxidation is disclosed in the vapour phase (a) of propylene, propane or isobutene by the instrumentality of molecular oxygen for receiving (meth)acrolein, and/or oxidation (b) of (meth)acrolein by molecular oxygen for receiving (meth)acryl acid, by the instrumentality of multiple-tubular reactor, contained: cylindrical reactor vessel, outfitted by initial material supply inlet hole and discharge hole for product, variety of reactor coolant pipes, located around the cylindrical reactor vessel and used for insertion the heat carrier into cylindrical reactor vessel or for removing the heat carrier from it, circulator for connection of variety loop pipeline to each other, variety of reaction tube, mounted by the instrumentality of tube reactor lattices, with catalyst. Also multiple-tubular reactor contains: variety of partitions, located lengthways of reaction tubes and used for changing heat carrier direction, inserted into reactor vessel. According to this heat carrier coolant flow is analysed and there are defined zones in reactor which have heat-transfer coefficient of heat carrier less than 1000 W/(m2·K); also reaction of catalytic oxidation is averted in the vapour phase in mentioned zones of reactor and reaction of catalytic oxidation is implemented in the vapour phase in reactor.

EFFECT: receiving of improved method catalytic oxidation in vapour phase which supplies effective removing of reactionary heat, excludes hot spot formation, and supplies effective receipt of base product.

3 cl, 6 dwg, 2 ex

FIELD: chemistry.

SUBSTANCE: invention concerns organic synthesis field, particularly method of obtaining benzoic acid (C6H5COOH, benzenecarboxylic acid) by catalytic oxidation of benzyl alcohol in hydrogen peroxide solution, as well as catalysts for method implementation, and method of obtaining catalysts. Catalysts of benzoic acid production is nanostructurised bifunctional metallocomplex catalyst acting as oxidation and interphase transport catalyst. It is a complex compound of the general formula Q3{PO4[W(O)(O2)2]4}, where: Q is quadruple ammonium cation [(R1)3N R2]+, where: R1 and R2 contain 8 to 24 carbon atoms. The invention concerns method of obtaining catalyst for benzoic acid production by dissolution of compounds containing phosphor and tungsten in hydrogen peroxide solution with added interphase transport catalyst compound, with phosphor-tungsten heteropolyacids of Keggin or Dawson structure are used as compounds containing phosphor and tungsten, dissolution is performed at the following mol ratio: hydrogen peroxide to tungsten [H2O2]/[W]=15-50, with further addition of quadruple ammonium cation - [(R1)3N R2]+ as interphase transport catalyst, where: R1 and R2 contain 8 to 24 carbon atoms. The invention also concerns method of obtaining benzoic acid by substrate oxidation in hydrogen peroxide in the presence of the catalyst described above.

EFFECT: increased efficiency of benzoic acid production process.

8 cl, 21 ex, 2 tbl, 1 dwg

FIELD: chemistry.

SUBSTANCE: invention concerns improved method of obtaining at least one product of partial propylene oxidation and/or ammoxidation, propylene selected out of group including propyleneoxide, acrolein, acrylic acid and acrylnitryl, where source substance is propane. Method involves a) at the first stage, homogeneous and/or heterogeneous catalysed dehydration and/or oxydehydration of raw propane in the presence and/or in the absence of oxygen, to obtain gas mix containing propane and propylene; and b) if required, separation of part gas mix 1 obtained at the first stage and its components other than propane and propylene, such as hydrogen, carbon monoxide, or transformation of this part in the other compounds, such as water, carbon dioxide, so that gas mix 1' containing propane and propylene and compounds other than oxygen, propane and propylene is obtained from gas mix 1; and at least one more stage c) heterogeneous catalysed ammoxidation and/or partial gas phase ammoxidation of propylene containing in gas mix 1 and/or gas mix 1' in gas mix 1 or gas mix 1' containing molecular oxygen of gas mix 2, where total C4-hydrocarbon content in gas mix 2 is < 3 volume %.

EFFECT: reduced process performance due to reduced output of target product and enhanced selectivity of carbon oxide generation at the second process stage.

50 cl, 10 ex

FIELD: chemistry.

SUBSTANCE: present invention pertains to improvement of the method of producing (met)acrylic acid or (met)acrolein using a multi-pipe reactor with a fixed bed. The reactor has several pipes, with at least one catalyst bed in the direction of the axis of the pipe. A heat carrier can regulate temperature outside the flow of the reaction pipe. In the reaction pipes, there is gas-phase catalytic oxidation of at least one type of oxidisable substance, propylene, propane, isobutylene and (met)acrolein by molecular oxygen or a gas, containing molecular oxygen. At the beginning of the process, the difference between the coolant temperature and the peak temperature of the catalyst is set in the interval 20-80°C, and during the process, peak temperature T(°C) of the catalyst in the direction of the axis of the pipe satisfies equation 1, given below: (equation 1), where L, T0, X and X0 stand for length of the reaction pipe, peak temperature of the catalyst in the direction of the axis of the pipe at the beginning of the process, the length up to the position which gives the peak temperature T at the input of the reaction pipe, and the length to the position which gives the peak temperature T0 at the input of the reaction pipe, respectively.

EFFECT: method allows for stable output of the target product, with high output for a long period of time, without reduction of catalyst activity.

3 dwg, 2 ex

FIELD: chemistry.

SUBSTANCE: present invention pertains to improvement of the method of producing (met)acrylic acid and complex (met)acrylic esters, involving the following stages: (A) reacting propane, propylene or isobutylene and/or (met)acrolein with molecular oxygen or with a gas, containing molecular oxygen through gas-phase catalytic oxidation, obtaining crude (met)acrylic acid; (B) purification of the obtained crude (met)acrylic acid, obtaining a (met)acrylic acid product; and (C) reacting raw (met)acrylic acid with alcohol, obtaining complex (met)acrylic esters, in the event that the installation used in any of the stages (B) and (C), taking place concurrently, stops. The obtained excess crude (met)acrylic acid is temporarily stored in a tank. After restoring operation of the stopped installation, the crude (met)acrylic acid, stored in the tank, is fed into the installation, used in stage (B), and/or into the installation used in stage (C). (Met)acrylic acid output of the installation used in stage (A) should be less than total consumption of (met)acrylic acid by installations used in stages (B) and (C).

EFFECT: the method allows for processing (met)acrylic acid, temporarily stored in a tank, when stage (B) or (C) stops, without considerable change in workload in stage (A).

2 ex

FIELD: chemistry.

SUBSTANCE: object of the present invention is to develop method for making catalyst to produce methacrylic acid by gaseous catalytic oxidation of metacrolein, isobutyl aldehyde or isobutyric acid. There is disclosed method for making catalyst to produce methacrylic acid by gaseous catalytic oxidation of metacrolein, isobutyl aldehyde or isobutyric acid, involving as follows: (a) the stage of mixing water and compounds, each containing any Mo, V, P, Cu, Cs or NH4, to prepare aqueous solution or dispersed compounds (further, both mentioned as a suspension); (b) the stage of drying suspension produced at the stage (a), to make dry suspension; (c) the stage of burning dry suspension produced at the stage (b), to make burnt substance; (d) the stage of filtrating mixed burnt substance produced at the stage (c) and water to separate aqueous solution and water-insoluble substance; and (e) the stage of drying water-insoluble substance produced at the stage (d) to make dry water-insoluble substance; and (f) the stage of coating the carrier with dry water-insoluble substance produced at the stage (e), with using a binding agent to make coated mould product, and (g) the stage of burning coated mould product produced at the stage (f) in inert gas atmosphere, in the air or with reducing agent added.

EFFECT: making catalyst with long life, high activity and selectivity.

8 cl, 9 tbl, 9 ex

FIELD: organic chemistry, medicine, pharmacology.

SUBSTANCE: invention relates to new derivatives of carbamic acid esters of the general formula (I):

and their pharmaceutically acceptable salts eliciting activity with respect to metabotropic glutamate receptors mGlu of group I that can be used for treatment of acute and/or chronic neurological disorders. In the general formula (I) R1 means hydrogen atom or (C1-C7)-alkyl; R2 and R2' mean independently of one another hydrogen atom, (C1-C7)-alkyl, (C1-C7)-alkoxy-group, halogen atom or trifluoromethyl; X means oxygen (O), sulfur (S) atom or two hydrogen atoms not forming a bridge; A1/A2 mean independently of one another phenyl or 6-membered heterocycle comprising 1 or 2 nitrogen atom; B represents group of the formula:

wherein R3 means (C1-C7)-alkyl and others; Y means -O-, -S- or a bond; Z means -O- or -S-; or B means 5-membered heterocyclic group of formulae: (a) , (b) , (c) or (d) . Also, invention relates to methods for preparing compounds and to a medicinal agent based on thereof.

EFFECT: improved preparing methods, valuable medicinal properties of compounds.

22 cl, 1 tbl, 2 sch, 78 ex

FIELD: chemistry of polymers, leather industry, chemical technology.

SUBSTANCE: invention relates to a method for preparing polymeric products that are used in processes for dressing leather or fur, in treatment and disinfection of natural and sewage waters. Method for preparing polymeric products involves the hydroxymethylation reaction of polyhexamethylene guanidine chloride with formaldehyde and arylation reaction of prepared product with aromatic compound comprising o-amino- or o-hydroxy-groups. The hydroxymethylation reaction is carried out in the presence of acetic acid or formic acid up to formation of trimethylol derivative of polyhexamethylene guanidine chloride. In some cases the arylation product is subjected for complex formation with transient metal salt or azo-coupling reaction with diazonium salt taken among group including sulfanilic acid, naphthionic acid, j-naphthyls, p-nitroaniline, 2,6-dichloro-4-nitroaniline. Invention provides simplifying, accelerating and enhancing the effectiveness of process in dressing leathers with derivatives of polyhexamethylene guanidine showing tanning effect, staining properties, flocculating capacity and high antibacterial activity.

EFFECT: improved preparing method.

3 cl, 1 tbl, 9 ex

FIELD: chemical technology.

SUBSTANCE: invention relates to a method for preparing disinfecting agent as derivative of polyhexamethylene guanidine. Method involves thermal polycondensation reaction of hexamethylenediamine and guanidine hydrochloride for two stages. At the first stage hexamethylenediamine is added to guanidine hydrochloride melt up to the molar ratio = 1:1 and mixture is subjected for control thermostatically up to ceasing ammonia evolving. At the second stage hexamethylenediamine excess is added to formed melt of polyhexamethylene guanidine chloride that is taken as measured its molar ratio with guanidine hydrochloride = 2:n wherein n means degree of polymerization that is calculated based on molecular mass of terminal groups of polyhexamethylene guanidine derivative obtained at the first stage by the following formula: n = [%Cl]*Mk/(35.45-[%Cl]*177.678) wherein %Cl means the relative content of chlorine by mass in derivative of polyhexamethylene guanidine; Mk means molecular mass of terminal groups of polyhexamethylene guanidine derivative and at Mk = 17.034 the relative content of Cl is determined in reaction mixture before addition of hexamethylenediamine excess, and at Mk = 215.382 the relative content of Cl is calculated in the composite of polyhexamethylene guanidine derivative formed at the second stage. Then the reaction mixture is subjected for control thermostatically at temperature 165-200°C up to ceasing ammonia evolving. The end product is prepared as polymer-analog of polyhexamethylene guanidine chloride. Invention provides reducing yield of the end product in water-insoluble fraction and to enhance bactericidal activity of disinfecting agent. Invention can be used in medicine and veterinary science, in treatment of natural and sewage waters, in processes for leather and fur tanning and in industrial and domestic conditions wherein bactericidal preparations are required.

EFFECT: improved preparing method.

1 tbl, 2 ex

FIELD: chemical technology, in particular production of formaldehyde derivatives.

SUBSTANCE: disclosed is continuous method for methylal production from aqueous solutions of formaldehyde and methanol in presence of tungstic heteropolyacid (silicotungstic and phosphotungstic acids) catalyst in rectifier reactor, wherein simultaneously chemical reaction is carried out and product is rectified or distilled from reaction zone. Further catalyst (heteropolyacid) is isolated from slop by water vaporization and recycled.

EFFECT: environmentally friendly method with decreased cost and energy consumption.

2 ex, 1 dwg

FIELD: chemical industry; methods and devices for reprocessing of the trifluotomethanesulfofluoride into the salt of the triluoromethanesulfo acid.

SUBSTANCE: the invention is pertaining to the improved method of production of the, which is the source product for the synthesis the trifluoromethanesulfofluoride derivatives of the triluoromethanesulfo acid, which are used in the thin organic synthesis, in production of the drugs, fungicides, extractants, catalysts, and also to the device for the method realization. The technical result of the invention is intensification of the process, the increase of productivity, the decrease of the losses of the trifluoromethanesulfofluoride at its reprocessing into the salt of the triluoromethanesulfo acid. The solution of the problem provides for feeding of the trifluoromethanesulfofluoride in its gaseous state into the mixture of the hydroxide (or oxide) the alkali-earth or the alkali metal with the water at the constant control of the pH value of the water mixture and the stopping delivery of the trifluoromethanesulfofluoride at рН=7. At that the trifluoromethanesulfofluoride is fed in the descending loop of the circulation of the water mixture at the volumetric ratio of the water mixture to the gas of not less than 6 and under the constant control of the contents of the trifluoromethanesulfofluoride in the effluent gases; feeding of the trifluoromethanesulfofluoride is terminated if its concentration in the effluent gases exceeds 0.5 % of their volume.

EFFECT: the invention ensures intensification of the process of reprocessing of the trifluoromethanesulfofluoride into the salt of the triluoromethanesulfo acid, the increased productivity, the decreased losses of the trifluoromethanesulfofluoride at its reprocessing into the salt of the triluoromethanesulfo acid.

3 cl, 4 ex, 1 dwg

FIELD: organic chemistry, medicine, cardiology.

SUBSTANCE: invention describes compounds of the formula (I): wherein R1 and R2 mean hydrogen atom (H), alkyl, fluorine (F), chlorine (Cl), bromine (Br) atom, alkoxy-group, -S(O)nR7, polyfluoroalkyl, polyfluoroalkoxy-group; R3 means Alk-R8, cycloalkyl; R8 means H, cycloalkyl, polyfluoroalkyl, phenyl or -OH; R4, R5 and R6 mean H or alkyl; R7 means alkyl. Also, invention relates to a method for synthesis of these compounds and a pharmaceutical composition possessing inhibitory activity with respect to Na+/K+ cellular exchange. Proposed compounds are suitable as anti-arrhythmic medicinal agents with a cardioprotective component used in prophylaxis of infarction and treatment of infarction and treatment of stenocardia. Compounds inhibit also pathophysiological process by prophylactic effect associated with development of disorders induced by ischemia, in particular, arising ischemia-induced cardiac arrhythmia and cardiac insufficiency.

EFFECT: valuable medicinal properties of compounds and pharmaceutical composition.

17 cl, 59 ex

FIELD: organic chemistry, detergents.

SUBSTANCE: invention relates to a novel mixture of alkoxylates possessing surface-active, moistening and cleansing properties of the formula: wherein PO means propyleneoxy link; ЕО means ethyleneoxy link; n has an average value in the range 1.6-3.3 per 2-ethylhexyl group; m has an average value in the range 3.0-5.5 per 2-ethylhexyl group and comprises less 1.5 wt.-% of unreacted 2-ethylhexanol. Indicated mixture is prepared by interaction of 2-ethylhexanol with propylene oxide at the first step, and at the second step propoxylated mixture is subjected for interaction with ethylene oxide, and amount of 2-ethylhexyl propoxylate is from 2 to 20 wt.-%. Also, invention relates to a method for preparing indicated mixture of alkoxylates wherein 2-ethylhexanol reacts with 1.6-3.3 mole of propylene oxide per a mole of 2-ethylhexanol in the presence of the propoxylation reaction catalyst at temperature from 110°C to 130°C at the first step wherein all amount of propylene oxide reacts. Then prepared mixture of propoxylates or mixture of propoxylates prepared after removal of unreacted 2-ethylhexanol is subjected for interaction at the second step with 3.0-5.5 moles of ethylene oxide per mole of 2-ethylhexanol in the presence of the ethoxylation reaction catalyst at temperature from 60°C to 180°C. Mixture of alkoxylates represents a good cleansing, surface-active substance and a moistening agent and can be easily biodegraded.

EFFECT: improved and valuable properties of mixture.

9 cl, 3 tbl, 5 ex

FIELD: synthesis of phosphorus-containing derivatives of organic compounds.

SUBSTANCE: invention relates to method of preparing polyphosphates of organic compounds, to mixture of polyphosphates of organic nitrogenous bases, and to use of polyphosphates and mixture of polyphosphates as fire retardants for plastics, preferably thermoplastics and, more particularly, polyamides and polyesters. Polyphosphates of organic compounds are prepared via exchangeable decomposition of mixture of phosphorus pentoxide and at least one organic nitrogenous base with a compound releasing water when decomposed under reaction conditions, the latter compound being used in such molar proportion that water would release in amount corresponding to essentially two moles of water per one mole of phosphorus pentoxide. Water-releasing compound can be compound forming, along with water, only volatile decomposition products and this compound can be selected from group including anhydrous oxalic acid, oxalic acid dehydrate, and formic acid. Exchangeable decomposition reaction is conducted at 100 to 250°C. Mixture of polyphosphates of organic nitrogenous bases is characterized by following properties: when heated to 320°C it looses less than 2% of its mass; pH value of its 10% water suspension exceeds 5 at 25°C, preferably from 5.2 to 7.7 and, more preferably, from 5.8 to 7; its solubility in water is less than 0.1 g and preferably less than 0.01 g per 100 mL water.

EFFECT: expanded synthetic possibilities.

6 cl, 5 ex

FIELD: chemical technology.

SUBSTANCE: invention relates to a method for synthesis of acetylene-unsaturated alcohol used in synthesis of vitamins and carotinoids. Method involves reaction of carbonyl compound with acetylene in the presence of ammonia and alkaline metal hydroxide wherein carbonyl compound represents methylethyl ketone, methylglyoxal dimethylacetal, 6-methyl-5-heptene-2-one, 6-methyl-5-octene-2-one, hexahydropseudoionone, 4-(2,6,6-trimethyl-1-cyclohexen-1-yl)-3-butene-2-one or 6,10,14-trimethyl-2-pentadecanone. Alkaline metal hydroxide is used in an aqueous solution wherein the molar ratio between this alkaline metal hydroxide and carbonyl compound is less 1:200. Method provides preparing acetylene-unsaturated alcohol with the high yield for the short reaction period.

EFFECT: improved method of synthesis.

11 cl, 5 tbl, 5 ex

FIELD: chemistry.

SUBSTANCE: invention pertains to the method of obtaining 7,7-methoxybicyclo[2,2,1]heptadiene-2,5, which is the initial reagent in the synthesis of tetramethoxyethylene, and is a powerful reducing agent and methylating agent. The method involves re-etherification of 7-tetrabutoxynorbornanediene (7-t-BuO-NBD) by methanol in the presence tetrachloromethane and Mo-containing catalyst Mo(CO)6, with subsequent oxidation of intermediate 7-methoxynorbornanediene by methylhypochlorite, formed in situ from tetrachloromethane and methanol. The reaction is carried out at 80-100°C for 2 hours and molar ratio [Mo(CO)6]:[t-BuO-NBD]:[CCl4]:[MeOH]=1:100:100÷200:100÷400.

EFFECT: method allows shortening the duration of the reaction, consumption of toxic reagents, simplification and reduction of expenses on the stage of separating the target product.

1 tbl, 1 ex

Up!