152 results about "Cyanohydrin" patented technology

1,2-diols can be obtained in good yields and in very high purity by a process of a)reacting a carbonyl compound of the general formula (I) with hydrocyanic acid to give the corresponding cyanohydrin,wherein R1 and R2 are each independently H, an optionally substituted straight-chain or branched C1-C18-alkyl radical, or an optionally substituted phenyl or C5-C6-cycloalkyl radical, b) subjecting the cyanohydrin obtained in process step a) to an acidic hydrolysis, and c) catalytically hydrogenating the 2-hydroxycarboxylic acid obtained from process step b) in the presence of a noble metal catalyst comprising ruthenium and rhenium.

A process for synthesizing L-valine from n-butanol and acetone cyanohydrin includes cyanation reacting under action of alkaline catalyst to obtain butanol cyanohydrin, ammonifying reacting on liquid ammonia, deammonifying, dewatering to obtain aminopentylonitrile, hydrolyzing in concentrated sulfuric acid, neutralizing, extracting, concentrating to obtain dl-aminopentyl amide, splitting, recrystallizing, dissolving in water, ion exchanging by cationic exchange resin, eluting by ammonia water, decoloring, dewatering, rinsing and drying.

The invention discloses an enzyme-linked immunosorbent assay method for multi-residue analysis of a cyano-containing pyrethroid pesticide, belonging to the technical field of immunoassay. The enzyme-linked immunosorbent assay method uses a coupled complex of hapten m-phenoxy benzal cyanohydrin succinate ester and ovalbumin as a coating antigen, samples of the cyano-containing pyrethroid and a polyclonal antibody of the m-phenoxy benzal cyanohydrin succinate ester are added, then the coating antigen and the cyano-containing pyrethroid to be detected are competed and reacted with the antibody, an enzyme-labeled secondary antibody is added to be combined with the fixed antibody, washing liquid is used for washing, developer is added, an enzyme-labeled instrument is used for detecting OD value, the OD value is compared with a standard curve of a standard product of the cyano-containing pyrethroid, and the concentration of the cyano-containing pyrethroid of the samples to be detected is calculated. The enzyme-linked immunosorbent assay method can accurately and sensitively detect the residues of the cyano-containing pyrethroid pesticide in the samples to be detected, the pre-treatment process of the samples is simple with less time-consuming, a large number of samples can be simultaneously detected, and the detection cost of the samples is far lower than the detection method of the traditional instrument; furthermore, the method of the invention has good stability and no radioactive pollution.

The present invention discloses flaxseed peptides having effects of lowering cholesterol and a preparation method thereof. The preparation method includes the following steps: flaxseed selecting and impurity removing, primary low-temperature and weak-acid water washing, primary beating, primary pectin lyase enzymatic digesting and degumming, primary papain, neutral protease, beta-glucosidase, alpha-cyanohydrin protein and hydroxynitrile lyases protein hydrolysate and cyanogenic glycoside decomposition reacting, ultrasonic high-temperature enzyme inactivating and detoxifying, and then centrifuging, nano-filtering, spray-drying, and cholesterol-lowering flaxseed peptide obtaining. The preparation method solves the effects of the flaxseed gum on the flaxseed proteolysis and removes cyanogenic glycosides and hydrocyanic acids in the products of the flaxseed peptides. The flaxseed peptide products are prepared for the first time, can be applied in the food and health-care food industries, and have broad business outlooks.

The invention provides a preparation method for D, L-phenylglycine and an analogue thereof. According to the method, benzaldehyde, an analogue thereof and hydrocyanic acid are adopted as raw materials and subjected to cyanidation reaction, and then 2-hydroxy-benzyl cyanide or 2-hydroxy-benzyl cyanide analogue (cyanohydrin for short) is generated. Cyanohydrin reacts with carbon dioxide and the aqueous solution of ammonia, and then 5-phenyl-hydantoin and an analogue thereof (hydantoin for short) are generated. hydantoin is successively subjected to steam stripping, alkaline hydrolysis, steam stripping, decolorization, neutralization, crystallization, washing, centrifuging, drying and the like to obtain D, L-phenylglycine and the analogue thereof. Compared with the prior art, the preparation method for D, L-phenylglycine and the analogue thereof can significantly and effectively reduce the pollution, and fewer inorganic salt by-products are generated. Meanwhile, the prepared D, L-phenylglycine and the analogue thereof are high in product yield and high in purity. Counted in benzaldehyde and the analogue thereof, the yield of D, L-phenylglycine and the analogue thereof is larger than or equal to 96%, and the product purity is larger than or equal to 99%. Meanwhile, the process flow is simple and feasible, so that the method is worthy of market popularization and application.

The invention discloses a method for synthesizing a glufosinate ammonium salt. The method comprises the following steps that (1) methyldiethoxyphosphine and n-butanol are used as raw materials to produce an intermediate I by hydrolysis and transesterification; (2) the intermediate I is subjected to a free radical addition reaction with acrolein cyanohydrin acetate to form an intermediate II; (3) the intermediate II is subjected to an aminolysis reaction with ammonia gas to form a mixture of an intermediate III and an intermediate IV; (4) the intermediate III and the intermediate IV are subjected to acid hydrolysis with hydrochloric acid to form an intermediate V; and (5) the intermediate V is neutralized, purified and crystallized to obtain the glufosinate ammonium salt. The method does not need to use toxic raw materials, avoids the large-scale use of ammonia water and ammonium chloride, not only greatly reduces the safety hazard, but also reduces the quantity of by-products and the amount of waste water generated, and the environmental protection risk is greatly reduced; and the purification process is simple, the product content and the yield coefficient are obviously increased,and the method is suitable for industrial scale production.

The invention discloses a method for synthesizing (R)-salmeterol. The method is implemented by taking p-hydroxy benzaldehyde as a raw material through the steps of carrying out a methylolation reaction on the p-hydroxy benzaldehyde so as to obtain prochiral aldehyde for protecting double hydroxide radicals in an acetal form; then, through taking (S)-BINOLAM.AlCl as a chiral catalyst, carrying out an asymmetric nucleophilic addition reaction so as to obtain a chiral cyanohydrin intermediate; and reducing the chiral cyanohydrin intermediate so as to obtain primary amine, reacting the primary amine with mesylate [6-(4 phenylbutoxy]hexane, and carrying out hydrolysis on the obtain product so as to remove protecting groups, thereby obtaining a final product (R)-salmeterol. In the invention, a chiral catalyst precursor (S)-BINOLAM can be reused; and the method has relatively high yield and relatively good enantioselectivity, and is short in synthetic route, simple and convenient in operation and low in cost.

The invention provides a cyanohydrins lyase and a preparing method and application thereof. Specifically, a mutational cyanohydrins lyase is obtained. Experiment results prove that the catalysis activity of the mutational cyanohydrins lyase is 200% or more that of wild mutational cyanohydrins lyase.

The invention discloses a separation and purification method for methionine hydroxy analogue synthesized through hydrolysis of cyanohydrins. The method comprises the following steps: carrying out ammonification and neutralization on hydrolysate obtained by hydrolysis of 2-hydroxy-4-methylthiobutyronitrile under the action of sulfuric acid and containing the methionine hydroxy analogue, ammonium sulfate and ammonium bisulfate, allowing ammonium sulfate to be precipitated through supersaturation and carrying out layering so as to obtain an organic layer I and a water layer I containing ammonium sulfate solid; concentrating the organic layer I so as to allow ammonium sulfate solid to be precipitated, carrying out solid-liquid separation, diluting obtained liquid through addition of water so as to obtain the commercial grade methionine hydroxy analogue, mixing the precipitated ammonium sulfate solid with the water layer I containing ammonium sulfate solid, and carrying out layering so as to obtain an organic layer II and a water layer II containing the ammonium sulfate solid; and subjecting the water layer II to solid-liquid separation and drying obtained solid so as to obtain commercial grade ammonium sulfate. The method provided by the invention is simple and easily practicable and can obtain the high-quality methionine hydroxy analogue and the commercial grade ammonium sulfate, and the recovery rates of the high-quality methionine hydroxy analogue and the commercial grade ammonium sulfate are more than 99%; and in the whole process of the method, no organic solvent is used, no waste water containing salt or organic matters is discharged, and cost and energy consumption are low.

The invention relates to a process for preparing acetone cyanohydrin and to a process for preparing alkyl methacrylates, in which an acetone cyanohydrin as can be prepared in accordance with the present invention is used.

The invention provides a method for synthesizing 17alpha-hydroxyprogesterone.17beta-cyano-5-androstene-17-alcohol-3,3-ethylene dihydroxy ketal (an intermediate II for short) is adopted as a raw material, and cheap cyclohexanone cyanohydrin is adopted as an inhibitor of a main impurity methyltestosterone. Due to the fact that a cyclohexanone cyanohydrin structure is similar to a D-loop structure in the molecular structural formula of the intermediate II and can replace a D loop to react with OH<1> in a Grignard reaction system, generated methyltestosterone is greatly reduced. Under the catalytic action of anhydrous lithium chloride or CuCl, the reaction temperature is reduced to -15 DEG C to -10 DEG C, and other generated impurities can be reduced at the low temperature. Therefore, the product quality is improved by controlling Grignard reaction conditions, the content of crude HPLC can reach 98% or above, and the total weight yield ranges from 84% to 88% and is improved by 10% to 14% compared with a traditional process.

A simple and easy-to-use method for producing a 2-hydroxyester compound using a cyanohydrin compound, as a raw material, is provided. A method for producing a 2-hydroxyester compound represented by the general formula (1) (provided that ethyl 2-hydroxy-4-phenylbutyrate is excluded), wherein an acid is introduced into a mixture of a cyanohydrin compound represented by the general formula (2), an alcohol, an organic solvent and water:(Chemical Formula 1)R1—CH(OH)—COOR2  (1)R1—CH(OH)(CN)   (2)wherein, R1 is a hydrogen atom, a substituted or unsubstituted aliphatic hydrocarbon group having 1 to 12 carbon atoms, which may contain an oxygen atom, a sulfur atom or a nitrogen atom, a substituted or unsubstituted alicyclic hydrocarbon group having 3 to 12 carbon atoms, which may contain an oxygen atom, a sulfur atom or a nitrogen atom, and a substituted or unsubstituted aryl group or aralkyl group having 3 to 14 carbon atoms, which may contain an oxygen atom, a sulfur atom or a nitrogen atom; and R2 is an alkyl group having 1 to 12 carbon atoms, which may contain an oxygen atom, a sulfur atom or a nitrogen atom.

The invention provides a method for preparing S-cyanohydrin. Cyanohydrin lyase is immobilized, and then a substrate is catalyzed to react to prepare S-cyanohydrin in a pure organic solvent. The method of immobilizing cyanohydrin lyase to prepare S-cyanohydrin is optimized, and optimized reaction conditions are obtained. Experiment results show that the optimized method for preparing S-cyanohydrin can efficiently prepare S-cyanohydrin, is high in product yield and stable in process, and the immobilized cyanohydrin lyase can be used repeatedly.

The invention discloses an application of n-butyllithium in catalyzing cyanosilylation reaction of ketone and silane. The n-butyllithium has high catalytic activity, low catalyst dosage and good substrate application range. After n-butyllithium, ketone and silane are mixed, the cyanosilylation reaction is carried out to obtain a cyanohydrin compound. The n-butyllithium reagent disclosed by the invention has the advantages of commercialization, easiness in obtaining, low cost, no need for a solvent, environmental friendliness and the like, has a very good catalytic effect on ketone, and is widein substrate application range. Commercial n-butyllithium is used for efficiently catalyzing the cyanosilylation reaction of ketone by using a relatively low dosage of catalyst.

The invention discloses an application of n-butyllithium in catalyzing cyanosilylation reaction of aldehyde and silane. The n-butyllithium has high catalytic activity, low catalyst dosage and good substrate application range, and after n-butyllithium, aldehyde and silane are mixed, cyanosilylation reaction is carried out to obtain a cyanohydrin compound. The n-butyllithium reagent disclosed by theinvention has the advantages of commercialization, easiness in obtaining, low cost, no solvent, environmental friendliness and the like, has a very good catalytic effect on aldehyde, and is wide in substrate application range. Commercial n-butyllithium can efficiently catalyze the cyanosilylation reaction of aldehyde by using a relatively low catalyst dosage.

This method discloses a zymochemistry method to synthesize optically active cyanohydrin compounds. By using hydroxyl-cyano lyase HNL---contained in almond, loquat seed, apple seed and Badawood seed to conduct catalytic reaction to obtain a new hydroxyl-cyano compound which can be used to synthesize various compounds such as thiamphenicol, florfenicol, etc..

The invention discloses a novel cyanohydrin enzyme and a method used for synthesizing chiral cyanohydrin, and particularly relates to the technical field of biology. The novel cyanohydrin enzyme is generated through the mutation of amino acid residues at the 103 site, the 128 site, the 141 site and the 220 site of a wild cyanohydrin lyase, wherein the amino acid residue at the 103 site is mutated into alanine, arginine, asparagine or asparaginic acid, and the amino acid residue at the 128 site is mutated into alanine, cysteine or glutamine. The novel cyanohydrin enzymeand the method used for synthesizing the chiral cyanohydrin have the advantages that a free drying method is adopted for replacing a stepped drying and concentration method in the prior art for processing semi-finished chiral cyanohydrin, in the actual application, the time required for preparing the chiral cyanohydrin is effectively shortened, the preparation difficulty of the semi-finished chiral cyanohydrin is reduced, and the method can be effectively applied to the industrial production while being applied to the laboratory preparation.

The invention provides a preparation device and a preparation method of cyanohydrin. The device comprises a feeder, a shell, an upper sealing head, a lower sealing head, reaction tubes and a liquid level meter, two ends of the shell are respectively connected with the upper sealing head and the lower sealing head, the feeder comprises a hydrocyanic acid feeding inlet, a first Venturi nozzle, a second Venturi nozzle, a catalyst feeding inlet and a static mixer; and a back plate is arranged in the shell, the reaction tube is filled with a filler, a position, close to the shell, of the upper sealing head is provided with a liquid distributor, and the lower sealing head is provided with a baffle plate. The preparation method comprises the following steps: material feeding, feeding of materials into the reactor, and material discharging, wherein the material feeding step is characterized in that a raw material 3-methylthiopropoanaldehyde is sent into a pipeline through the first Venturi nozzle, a raw material hydrocyanic acid is sent into the pipeline from the hydrocyanic acid feeding inlet, the raw materials enter the liquid distributor, go through the distribution holes of the liquid distributor and are sent into the corresponding reaction tubes, the reaction tubes are filled with the filler, and the obtained material is discharged after a reaction. The reaction yield is 99.99-99.998%.

The invention discloses a pyrethroid compound having a structure represented by general formula (I). The invention also discloses a preparation method of the compound, and uses of the compound. The method comprises the following steps: utilizing a chiral adjuvant induced asymmetric syntheses technology to construct a novel pyrethroid key intermediate chiral carboxylic acid, and condensing the chiral carboxylic acid with active molecules comprising plant essential oil micromolecules, substituted cyanohydrin, fluorine-containing benzyl alcohol and the like to obtain the novel pyrethroid compound. The pyrethroid compound is used for preparing pesticides or pesticide active components for killing important agricultural pests comprising cotton bollworms, diamondback moths, aphids, beet armyworms, armyworms and the like, and healthy pests comprising houseflies, Culex pipiens pallens and the like, and can be widely used for the comprehensive control of crop pests.

The invention discloses a method for clean and stable storage of cyanohydrin products. A recyclable heterogeneous stabilizer substitutes a traditional inorganic acid to serve as a cyanohydrin stabilizer. According to short, medium and long term different storage duration requirements, the content of moisture and hydrocyanic acid components in cyanohydrin and impurity removal are selectively adjusted to reduce unnecessary stabilization process operations and waste of hydrocyanic acids, the stabilizer and the like serving as stable resources as far as possible while stable storage of cyanohydrinin required storage duration is realized. By use of the heterogeneous stabilizer, cyanohydrin contamination caused by inorganic acid can be avoided, recyclability is realized, and cleanness and energy saving in storage of the cyanohydrin products are achieved.

The invention relates to a method for producing chiral α-hydroxycarboxylic crystalline acids consisting in transforming cyanhydrins (R) or (S) into α-hydroxycarboxylic acids (R) or (S), respectively by enzymatic hydrolysis in the presence of Rhodococcus erythropolis NCIMB 11540.

The invention provides a preparation method of 1-cyano-2-allyl acetate. The preparation method comprises an esterification reaction and distillation. Acrolein cyanohydrin and liquid acetic anhydride are subjected to the esterification reaction in the presence of a catalyst and inorganic acid to prepare a reaction solution containing ACA, an ACA product is obtained after distillation, and the esterification reaction further comprises the step of introducing gaseous acetic anhydride into a reaction system. The invention further provides a preparation device of 1-cyano-2-allyl acetate. Accordingto the method and the device, acetic anhydride is ingeniously divided into two parts to be fed, one part is separated out to serve as acetic anhydride steam which is fed into an esterification reaction tower from the bottom of the tower, heat required by reaction can be provided, acetic acid can be effectively blown off, the esterification reaction can be accelerated through effective removal of acetic acid, and the reaction efficiency is improved. The device is characterized in that a conductivity meter is arranged in the esterification reaction tower to monitor the reaction process on line,so that the timeliness and effectiveness of reaction process control are guaranteed.

The present invention primarily relates to a process for producing certain phosphorus-containing cyanohydrin esters of formula (I) and the use thereof for producing glufosinate / glufosinate salts. The present invention further relates to a process for producing glufosinate / glufosinate salts.

The invention provides a process for synthesizing methyl methacrylate from ethanol, and belongs to the technical field of methyl methacrylate synthesis. The process comprises the steps of taking ethanol and CO as raw materials, carrying out carbonylation reaction under the action of a catalyst to synthesize propionic acid, carrying out esterification reaction on propionic acid and methanol under the action of a strong acid catalyst to generate methyl propionate, and carrying out gas-phase aldol condensation reaction on methyl propionate and formaldehyde under the action of an acid-base catalyst to obtain a methyl methacrylate product. The existing MMA production technology such as an acetone cyanohydrin method (ACH), an isobutene method (C4 route) and an ethylene method belongs to production process technology of the petroleum route, the process provided by the inventiontakes ethanol as a raw material and is an MMA production technology of the coal-based route, and the development of the MMA production technology of the coal-based route has important practical significance for the current situation of less-oil and more-coal energy.

The invention belongs to the technical field of industrial water treatment and in particular relates to a method for measuring the polyepoxysuccinic acid content of circulating cooling water by a pinacyanol chloride spectrophotometric method. The method particularly comprises the following steps of: preparing a group of polyepoxysuccinic acid solution at the concentration of 0 to 1.5 mg / L; adding borax-sodium hydroxide buffer solution with the pH value of 9.40 and pinacyanol chloride standard solution into the polyepoxysuccinic acid solution; developing for 5 minutes; measuring the absorbance at the position of 600 nm by using a spectrophotometer; deducting blank absorbance from the absorbance of the solution to form linear relationship between the absorbance of the solution and the polyepoxysuccinic acid concentration, wherein distilled water serves as blank; and obtaining the polyepoxysuccinic acid concentration in a circulating cooling water system through a standard curve. The method has the advantages of simpleness, convenience, easiness in operation, capacity of measuring the dirt dispersion agent polyepoxysuccinic acid content of the circulating cooling water quickly and accurately and the like. By the test method, the basis can be provided for quantitatively adding the polyepoxysuccinic acid scale and corrosion inhibitor of the industrial circulating cooling water; medicament cost can be effectively reduced; the using efficiency of the medicaments can be improved; and the circulating cooling water system can operate normally.

The invention relates to a synthetic method for m-phenoxybenzoic armour cyanhydrin succinic acid ester, and belongs to the technical field of biochemistry industry. By utilizing m-Phenoxybenzaldehyde as the raw material, the synthetic method includes two steps of reactions including compounding m-phenoxy armour cyanhydrin primarily and compounding the m-phenoxybenzoic armour cyanhydrin succinic acid ester subsequently. By utilizing simple synthetic processes, the invention successfully compounds the m-phenoxybenzoic armour cyanhydrin succinic acid ester which is a derivate of the m-phenoxy armour cyanhydrin. After the post treatment, the m-phenoxybenzoic armour cyanhydrin succinic acid ester with a purity of more than 99 precent can be used as standard. The invention provides a convenient way for future test and research on the enzyme-linked immunoassay of pyrethroids containing cyano group, and satisfies the needs of the relative researchers both domestic and abroad.

The invention discloses a method for preparing 17 beta-cyano-17 alpha-hydroxy-9-dehydroandrostenedione. The method comprises the following steps: (1) dispersing 9-dehydroandrostenedione (I) and acetone cyanohydrin (II) into an organic solvent; (2) carrying out a cyanohydrination reaction on the obtained mixed raw material liquid in a tubular reactor filled with strongly basic ion exchange resin, and (3) carrying out post-treatment on the material liquid after the cyanohydrination reaction to obtain 17beta-cyano-17alpha-hydroxy-9-dehydroandrostenedione (III), the reaction formula of which is shown in the specification.

The present invention provides a new electroless gold plating bath that can comprehensively improve the plating stability, the appearance after plating and the plating speed. The electroless gold plating bath of the present invention contains a water-soluble gold compound, a reducing agent, a complexing agent, and a stabilizer, wherein the stabilizer is a cyanohydrin compound represented by the following formula. In the formula, R1 and R2 are the same or different and represent a hydrogen atom, a silyl group, or an alkyl group or an aryl group which may be substituted with a substituent.

The invention discloses a preparation and purification method of methacrylamide. The method comprises the following steps: hydrolyzing and dehydrating by concentrated sulfuric acid to generate methacrylamide sulfate based on acetone cyanohydrin as a main raw material; neutralizing the methacrylamide sulfate by ammonia gas or ammonia water; circularly applying the neutralized centrifuged mother liquor; and purifying the methacrylamide crude product containing ammonium sulfate by sublimating, thereby obtaining the pure methacrylamide. According to the process, the mother liquor can be circularly applied so as to greatly reduce the discharge of salt-containing acid-containing sewage and avoid the environment pollution, reduce the dissolving of the methacrylamide in the mother liquor and improve the yield of the methacrylamide; and the purity of the obtained pure methacrylamide can be more than 99%, and the yield is more than 90%.