The method of obtaining salts of acids orthocarbonate

 

(57) Abstract:

Usage: as intermediates and in printing. Entity: an improved method of obtaining salts orthocarbonate acids of the formula R-C(OH)(OMe)2where R is phenyl, furyl, R1-CH=CH-, CH3-(CH=CH)2- That ; Me - Na, K; R1- Ph, furyl. Reagent 1: carboxylic acid of the formula R - CO(OH) where R is the specified value. Reagent 2: aqueous solution of potassium hydroxide or sodium concentration of 6 - 8 mol/l reaction Conditions: reagent 1 is treated with reagent 2 before the formation of a thick precipitate in the presence of diethyl ether in a volume ratio to the reaction mass, respectively(1 - 1,7) : (2,1 - 2,36), at 30 - 50C to remove excess alkali. table 2.

The invention relates to organic chemistry, namely to new ways of obtaining salts orthocarbonate acids, or alcoholate hem-triolo having the structural formula R-Me where R is phenyl, furyl, Rl-CH= CH-, CH3-(CH= CH)2- CH= Me - Na, K; Rlis phenyl, furyl, used as an intermediate reagents, as well as having application in the printing industry for the regeneration of aluminum foil.

A method of obtaining salts orthocarbonate acids by mixing the organic acid duhf the Aliyevs salt orthobenzoquinone acid. The closest analogue is the way, which consists in prilivnyi concentrated alkali to a heterogeneous mixture of organic acid-water before the formation of a copious precipitate of the product with the subsequent removal of excess alkali in the filter SCHOTT. In both cases, the product is formed by the following reaction equation: R-O R - R-Me

The disadvantage of analog is bad achievement purity primary product from alkali, because the concentrated alkali, which represents the main component of the reaction mixture cannot be separated by any solvent. Water or aqueous solvents decompose the product by the reaction of R-Me R- + MeOH

When washing orthocarbonate salt aqueous alkali solution with a concentration of less than 6 N. salt is decomposed at a higher concentration of alkali salt in the solution is sustainable.

The aim of the invention is to obtain a pure product with a higher yield by separating it from the reaction mixture directly in the flask during its formation.

This goal is achieved by the fact that the aqueous alkali solution with a concentration of 6-8 M/l is added to the carboxylic acid in the presence of diethyl ether in a volume ratio to the total volume of the reaction mixture (1-1,7) the cluster of boiling ether. Deviation from these conditions leads to a change in the direction of the reaction, resulting in the formation (with a low content of alkali salt of carboxylic and not orthocarbonic acid. A smaller content of the ether does not provide separation of the product from the reaction mixture, and the more inappropriate the flow of solvent. If all these relationships formed orthocarbonate salt is separated from the alkaline reaction mass and enters the ether layer from which is extracted by known methods.

Described by provides the potassium and sodium salts orthocarbonate acids specified patterns of high purity with a yield up to 90% , stable during storage. The spectral analysis is performed and other methods. The table shows the results of retrieval orthocarbonate salts of the inventive method.

P R I m m e R. Donationtree. 5.6 g (0.05 M) pyrolysis acid is stirred with 50 ml of water, resulting in a suspension of crystals of the acid in water. To this mixture is added dropwise with stirring, poured separately prepared solution of 40 g (1.0 M) of NaOH in 100 ml water. First, the reaction mixture becomes homogeneous as a result of formation of sodium salt pirolisi which take place all more white precipitate. By the end of prilipanie alkali reaction mass is dense hard mix a lot. The temperature of the reaction mass is raised to 70-80aboutC. Water bath to regulate the temperature of the mixture within 40 10aboutC. At the end of prilipanie alkali mixture is allowed freely to cool for 1-2 h, after which it is poured 100 ml of diethyl ether and left for 1 h without stirring. During this time there is delamination of the reaction mass, and the crystalline product enters the upper ether layer, forming a heterogeneous mixture in air. Separating the lower liquid layer represents the excess alkali in aqueous solution. Using a pipette, 50 ml of the lower layer is removed from the flask, a suspension of the product in ether, transferred to a glass filter and squeeze the product from ether residues and aqueous alkali. The crystalline product is transferred into a flask with a new portion 100 ml of ether, stirred and left for 1 h to separate the residue aqueous alkali, which removes similarly, a pipette, and the product again press on the filter SCHOTT. The obtained sodium salt ostoperosis acid dried in a thermostat at 50aboutWith and then for 2 h at 130aboutC. the Yield of 7.7 g, or 90% of theoretical is prohibited, % : From 34.5; H 2,3; Na 26,4.

The IR spectrum of the product contains the line that matches he3800 cm-1. Potentiometric titration of an aqueous solution of the product installed basic substance content of 98% .

For other articola listed in the table, the synthesis is carried out similarly.

When introduced into the reaction mixture of ether is less than 0.7 to volume of the mixture effect separation of the mixture will not occur, and the introduction of ether in a quantity greater than 1: 1 is impractical high consumption of solvent. (56) USSR Author's certificate N 1461642, class B 41 N 3/06, 1989.

Journal of General chemistry 58, 1988, No. 4, S. 987.

The METHOD of OBTAINING SALTS ORTHOCARBONATE ACIDS of General formula

R-Me

where R is phenyl, furyl;

R1-CH= CH-, CH3-(CH= CH)2-,

CH2= C-CH3, And Me is Na, K,

where R1is phenyl, furyl, processing carboxylic acid of General formula

R-O

where R has the above meaning,

aqueous solution of potassium hydroxide or sodium concentration of 6 - 8 mol before the formation of a thick precipitate by the addition of ether, removing excess alkali, wherein the process is conducted at 30-50oWith as diethyl ether used in a volume ratio with reaction mass

 

Same patents:

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

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

Up!