68results about "Oxygen-containing compound preparation" patented technology

The invention discloses a synthesis method of 2, 4, 5-trifluorophenylacetic acid, which comprises the following steps: by taking cheap and easily available o-chloronitrobenzene as a raw material, reacting with sodium nitrate in a sulfuric acid and trifluoroacetic acid system, separating generated 2, 4-dinitrochlorobenzene through melt crystallization, and continuing to synthesize 2, 4-dinitrochlorobenzene in methyl chloroacetate to obtain 2, 4, 5-trifluorophenylacetic acid. The method comprises the following steps: carrying out indirect aromatic nucleophilic substitution reaction on 2, 4-dinitrophenylacetic acid under the condition of sodium hydride to generate 5-chloro-2, 4-dinitrophenylacetic acid methyl ester, separating, carrying out fluorination reaction on the 5-chloro-2, 4-dinitrophenylacetic acid methyl ester and potassium fluoride under the action of a phase transfer catalyst, carrying out rectification separation to obtain 2, 4, 5-trifluorophenylacetic acid, and carrying out hydrolytic acidification on the 2, 4, 5-trifluorophenylacetic acid in a sodium hydroxide aqueous solution to obtain 2, 4, 5-trifluorophenylacetic acid. And the process route is safer, more environment-friendly, more efficient and lower in cost.

The invention discloses a recovery process of waste PET (polyethylene glycol terephthalate), which comprises the following steps: dissolving waste PET by using a good solvent, dropwise adding into cold methanol, precipitating, filtering, separating, drying, and hydrolyzing the waste PET by using a low-concentration sodium hydroxide aqueous solution, so that the PET can be effectively hydrolyzed at a relatively low temperature (25-40 DEG C), the reaction conditions are mild, the reaction time is short, the yield is high, and the recovery process is suitable for industrial production. The yield of the product TPA is up to 99%, the product TPA is easy to separate, and the solvent can be recycled.

The invention discloses a method for depolymerizing polyester. The method comprises forming a polyester comprising the following components (a), (b) and (c): (a) a polyester, (b) one or more basic compounds selected from the group consisting of alkali metal hydroxides, alkali metal carbonates, alkali metal bicarbonate salts, alkaline earth metal hydroxides, alkaline earth metal carbonates and alkaline earth metal bicarbonate salts, and (c) and a step of depolymerizing the polyester in the mixture of a solvent containing at least one of an alcohol-based solvent and a ketone-based solvent. The temperature of the mixture at the time when the mixture containing the total amount of the polyester, the basic compound, and the solvent is formed is 75 DEG C or less. The ratio of the amount of the polyester to the amount of the solvent is 0.2-20 by mass.

To provide a method for producing a cyclohexanedicarboxylic acid-based compound which can simply obtain a cyclohexanedicarboxylic acid-based compound such as DMCD from a polymer having a terephthalic acid skeleton at a sufficient yield at low cost.SOLUTION: A method for producing a cyclohexanedicarboxylic acid-based compound includes performing exchange reaction of an ester group or an amide group and alcohol or water in the presence of a catalyst A, and nuclear hydrogenation reaction in the presence of the catalyst A and a nuclear hydrogenation catalyst B, on a polymer having a terephthalic acid skeleton containing an ester group or an amide group, and thereby obtaining a cyclohexanedicarboxylic acid or a cyclohexanedicarboxylic acid ester, wherein the catalyst A containing at least one selected from Group 2 elements (excluding strontium) and Group 3 elements, and the nuclear hydrogenation catalyst containing at least one selected from a catalyst containing ruthenium, and a platinum-carrying catalyst in which platinum is carried on silica are used.SELECTED DRAWING: None

Depolymerization of polyalkylene terephthalate resin using Alcosilis, providing a superior depolymerization method. [Solution] The method for depolymerizing a polyalkylene terephthalate resin according to the present disclosure is a method for depolymerizing a polyalkylene terephthalate resin by alcoholization of the polyalkylene terephthalate resin, wherein the polyalkylene terephthalate resin includes a polybutylene terephthalate resin, and the alcohol used for alcoholization contains tetrahydrofuran in a proportion of more than 0 ppm by mass and 100,000 ppm or less by mass.

The invention relates to a method for synthesizing (R)-3-methylheptanoic acid. According to the method, the application range of steroid sapogenin degradation waste is further expanded. According to the method disclosed by the invention, the (R)-3-methyl-heptanoic acid can be conveniently obtained by taking the (R)-4-methyl-gamma-butyric acid lactone obtained by degrading steroid sapogenin as a raw material. According to the method provided by the invention, the use of highly toxic and controlled reagents is avoided, high-risk reactions such as hydrogenation in the prior art are avoided, and the method is mild in reaction condition and low in synthesis cost. Meanwhile, the utilization rate of steroid sapogenin resources is increased, and waste generated in the utilization process of the steroid sapogenin resources is reduced.

The invention discloses hump conjugated linoleic acid, a hump conjugated linoleic acid microcapsule and a preparation method and application of the hump conjugated linoleic acid microcapsule, and belongs to the technical field of deep processing of hump fat. According to the method, petroleum ether is used as a solvent, crude fat is extracted from hump fat through a Soxhlet extraction method, NaOH-ethanol is used for saponifying the crude fat, then a low-temperature crystallization method is combined with a urea adduction method, and finally, the conjugated linoleic acid is effectively separated and purified. The determination of the free radical scavenging ability of DPPH and ABTS shows that the obtained CLA has oxidation resistance. Extracted and purified conjugated linoleic acid is used as a core material, whey protein isolate and maltodextrin are selected as wall materials, an emulsion is prepared, and microcapsule powder is prepared by a direct vacuum freeze-drying method. Experiments show that the prepared conjugated linoleic acid microcapsule has a complete structure and good thermal stability.

To improve the recovery rate of alcohol, which is a constituent monomer of polyester resin, in a method for decomposing polyester resin using high-temperature water. [Solution] A method for decomposing polyester resin, comprising step (i) of hydrothermally treating polyester resin in the presence of polyamide resin, wherein step (i) includes proceeding with hydrolysis of the polyester resin at a temperature of 150°C or higher.

The invention relates to novel salts of N-substituted 2-amino-4-methylpyrimidine-5-yl-carboxylic acids having the formula (I), where the values of the radicals are disclosed in the claims, and the use of said salts as a growth stimulator for plants and fungi. The invention further relates to embodiments of methods for producing N-substituted 2-amino-4-methylpyrimidine-5-ylcarboxylic acids having the formula (I). The technical result is the production of novel salts of N-substituted 2-amino-4-methylpyrimidine-5-yl-carboxylic acids having the formula (I) which exhibit improved plant growth stimulator properties.

The invention relates to a method for removing heavy metals in borneol. Specifically, the invention provides a method for reducing the content of heavy metals in borneol, and the method comprises the following steps: (1) mixing a borneol crude product with an organic solvent to obtain a borneol crude product solution; and (2) adding propolis and activated carbon into the borneol crude product solution obtained in the step (1), stirring, filtering, concentrating the filtrate under reduced pressure, crystallizing and filtering the obtained concentrated solution, and drying the obtained solid to obtain the borneol pure product, thereby reducing the content of heavy metals in the borneol. The method provided by the invention can effectively reduce the content of heavy metals such as arsenic, lead, mercury, cadmium and copper in the borneol, so that the heavy metals in the borneol can be effectively controlled, and the application value of the borneol is improved.

This invention provides a novel method for manufacturing fluorinated carboxylate compounds, for producing formula (P1): (B 1f ) mp (A) 1 ) np [B] 1f RfCOO; Rf is a hydrocarbon group having one or more fluorine atoms; A 1 It is a group other than H; mp is (A 1 The valence of () × np and is 1 or 2; np is mp / (A 1 The valence of A is 1; 1 The method of manufacturing a compound having a valence of 1 or 2 includes: making formula (S1): (B 1f (R) 1 ) [R 1 The compound shown is an organic group and is related to formula (S2): (A 1 ) ms2 (B) 2 ) ns2 [B] 2 It is OH, CO3 or HCO3; ms2 is (B 2 (valence) × ns2 / (A) 1 The valence of ns is 1 or 2; ns2 is (A 1 (value) × ms² / (B) 2 The reaction of the compound or its hydrate shown in the figure (with a valence of 1 or 2) is a step A.

The application discloses a polyester degradation method. Specifically, the polyester degradation method comprises the following steps: degrading the polyester under the action of a carboxylic acid and a catalyst, namely, the polyester is degraded; the polyester comprises repeating units formed by a dibasic carboxylic acid and a dihydric alcohol; and the catalyst is a Lewis acid and / or a sulfonic acid organic acid. The degradation method has wide application range, the obtained product dicarboxylic acid is simple to separate and can be used for resynthesis of the polyester, the catalyst can be recycled and reused, the obtained product dihydric alcohol dicarboxylic acid ester can be reduced by hydrogenation to form a carboxylic acid, and the carboxylic acid and the catalyst in the degradation solution are repeatedly used for degradation of the polyester, so that the industrial benefits of the polyester degradation are maximized.

The application discloses a preparation method of 2-ethyl-2-methyl pentanoic acid, wherein in the process of preparing a key intermediate 2-cyanopentanoate (compound B), compound A is removed by using an alkali extraction method, high-purity compound B is separated by using rectification (a yield of 20% and a purity of 98%), and the operation process is simple. In the preparation method, reagents used are sodium methoxide, sodium hydroxide, sulfuric acid, sodium hydride and sodium nitrite, the reagents are simple, the danger is relatively small, and the experimental operation is relatively safe. In the preparation method, the post-treatment processes of alkylation, hydrolysis, deacidification and cyano hydrolysis do not use a chromatographic column purification process, and a conventional extraction distillation operation is adopted, so that the output of unit volume of instrument equipment is high.

The utility model belongs to the technical field of separation, and particularly relates to an ethyl acetate and butanone separation device, which comprises a butanone separation tower, an ethanol separation tower and an ethyl acetate separation tower which are connected in sequence, in the utility model, the tower top produced liquid of the ethyl acetate separation tower returns to the butanone separation tower, so that the purity of the product can be further improved; the gas phase of the butanone separating tower is used as a heat source of a reboiler at the bottom of the ethyl acetate separating tower, the gas phase at the top of the ethyl acetate separating tower is used as a heat source of a reboiler at the bottom of the ethanol separating tower, heat coupling can be realized between the rectifying towers with different operating pressures, the energy consumption in the rectifying and separating process is further reduced, and the method has higher operability.

The present invention relates to a novel method for isolating capsanthin and several other carotenoids from paprika oleoresin, a concentrated extract of paprika fruit (Capsicum annuum). In another aspect, the invention relates to the use of mild non-aqueous and aqueous saponification methods for isolating highly pure capsanthin and other carotenoids from paprika oleoresin at temperatures of about 20-50°C. In another aspect, the invention relates to a saponification method that results in a crystalline mixture of capsanthin, β-carotene, β-cryptoxanthin, and zeaxanthin, which can be separated by solvent extraction and crystallization to obtain highly pure capsanthin and other carotenoids.

The invention provides an olefine aldehyde intermediate and a synthetic method thereof, and a synthetic method of conopomorpha sinensis sex pheromone, and belongs to the field of compound synthesis. According to the synthesis method of the olefine aldehyde intermediate, provided by the invention, 1, 5-pentanediol is taken as a raw material, and the high-yield olefine aldehyde intermediate is obtained through transesterification, first oxidation reaction, Wittig reaction and Sagsa oxidation reaction; the yield of the olefine aldehyde intermediate can be further improved by limiting a catalytic system and an auxiliary agent of the Sagsa oxidation reaction. Results of the embodiment show that the synthesis method provided by the invention does not adopt alkyne compounds, the yield of the product in the Sagassa oxidation reaction stage can reach 81%, the total yield of the obtained olefine aldehyde intermediate can reach 48.5%, the sex pheromone of conopomorpha sinensis prepared by adopting the olefine aldehyde intermediate can reach 39.8%, and the yield is high.

The invention provides a method for depolymerising a phenolic polymer, the method comprising reacting the phenolic polymer with dimethylsulphoxide (DMSO) and a hydrogen halide. The phenolic polymer may be selected from the group consisting of lignin and derivatives thereof. The hydrogen halide may be HBr. The quantity of hydrogen halide per gram of phenolic polymer may be from 30 mmoles to 70 mmoles. The quantity of DMSO per gram of phenolic polymer may be from 0.1 mole to 1 mole. The reaction may be performed at a temperature of from 100 to 120 °C. The reaction may be carried out for between 10 h and 14 h. The product of the reaction may comprise vanillin.

The present invention relates to compounds of formula (I) as perfume precursor compounds. In particular, the present invention relates to a method for releasing a compound of formula (I) that is a carbonyl of formula (II), a formate of formula (III), and / or an alcohol of formula (IV) by placing the compound of formula (I) in an environment where it is oxidized. Furthermore, the present invention relates to perfume compositions and consumer perfume products containing at least one compound of formula (I).

The invention discloses a preparation method of methylallyl alcohol, which comprises the following steps: adding tricarboxylate into a reaction kettle, adding water for dissolving, heating and refluxing; dropwise adding methyl allyl chloride, and controlling the reaction temperature; cooling and filtering to obtain tricarboxylate solid and filtrate for later use; adding the tricarboxylate solid into a sodium hydroxide aqueous solution for reflux hydrolysis, cooling and layering to obtain methylallyl alcohol and tricarboxylate, and after separation, combining the tricarboxylate with the filtrate for recycling. The polycarboxylate obtained after esterification of the ternary carboxylate has small solubility in a solution, and an esterification product is a precipitate and can be naturally separated out; the esterification reaction can be carried out even under the condition of no catalyst, and the reaction is simple and rapid; then, the polybasic carboxylic ester can be separated through simple filtration, so that the emulsification phenomenon of the carboxylic ester in a water layer is overcome; and hydrolyzing the polybasic carboxylic ester to obtain corresponding alcohol and tricarboxylate, rectifying the alcohol to obtain the product methylallyl alcohol, and recycling the tricarboxylate.

The invention relates to the field of organic synthesis, and particularly discloses a preparation method of kung-fu acid. Comprising the following steps: carrying out an addition reaction on 3-methyl-1-butene and 1, 1, 1-trichlorotrifluoroethane under the action of a catalyst to obtain 2, 2, 4-trichloro-1, 1, 1-trifluoro-5-methylhexane, carrying out an elimination reaction under a strong alkaline condition to obtain 2-chloro-1, 1, 1-trifluoro-5-methyl-2, 4-hexadiene, carrying out a '1 + 2' cycloaddition reaction on the 2-chloro-1, 1, 1-trifluoro-5-methyl-2, 4-hexadiene and a phosphorus ylide reagent to obtain 2-chloro-1, 1, 1-trifluoro-5-methyl-2, 4-hexadiene. And finally, saponifying and acidifying the kung-fu acid methyl ester to obtain the product kung-fu acid. The process is simple to operate, the raw materials are cheap and easy to obtain, the solvent can be recycled, the conversion rate is high, impurities are few, and the method is more suitable for industrial production.

The invention belongs to the technical field of organic synthesis, and particularly relates to a method for synthesizing 3, 4-difluoro-2-methoxyphenylacetic acid without transition metal catalysis, which comprises the following steps: by taking 2, 3, 4-trifluoronitrobenzene as an initial raw material, carrying out substitution, methylation, reduction, Sandmeyer reaction, cross coupling, hydrolysis and other reactions, and synthesizing the 3, 4-difluoro-2-methoxyphenylacetic acid without transition metal catalysis. The total yield is 55.6%, and the content of the refined 3, 4-difluoro-2-methoxyphenylacetic acid reaches 99% or above. The method has the advantages of mild reaction conditions, simple operation, high reaction yield, easy purchase of used reagents and instruments, low cost, no need of any transition metal catalysis, and feasibility in specific practical application.

The present invention relates to a solid material based on BHET having a crystalline form with a specific X-ray diffraction pattern, a method for its preparation, a composition comprising said material, and the use of said composition for preparing polyesters.

The invention discloses a Co-coated Ni3S2-x catalyst with monatomic Co anchored in S vacancy and a preparation method and application thereof, and the synthesis method comprises the following steps: adding thiourea into deionized water, fully dissolving and uniformly dispersing, immersing foamed nickel into the mixed solution, and preparing Ni3S2 through a hydrothermal method. The preparation method comprises the following steps: carrying out argon plasma bombardment on Ni3S2 to prepare Ni3S2-x containing S vacancies, dipping Ni3S2-x in an aqueous solution containing Co (NO3) 2.6 H2O, and calcining in an H2 / Ar atmosphere to anchor monatomic Co on the S vacancies to prepare Co (at) Ni3S2-x. The Co-coated Ni3S2-x catalyst prepared by the invention can be used for converting PET derivative ethylene glycol into high-value formic acid at normal temperature and normal pressure.

To provide a technique capable of inexpensively decomposing a polyester resin without using an expensive useful chemical substance as a material.SOLUTION: A method for decomposing a polyester resin brings a polyester resin into contact with a solid of an oxide or a hydroxide having a standard oxidation reduction potential in the water higher than a standard oxidation reduction potential of water in the water, and hydrolyzes the polyester resin.SELECTED DRAWING: Figure 1

This invention provides a method for preparing 3-cyanomethyl-5-methylbenzamide, belonging to the field of pharmaceutical preparation technology. The method uses 5-methylisophthalic acid as a raw material, preparing 5-methylisophthalate diester via diesterization, followed by selective reduction to obtain 3-hydroxymethyl-5-methylbenzoic acid ester, which is then hydrolyzed to obtain 3-hydroxymethyl-5-methylbenzoic acid. Subsequently, a hydroxymethyl substitution reaction and amidation are performed to obtain 3-substituted methyl-5-methylbenzamide, which is finally prepared by cyanolation to obtain the target product, 3-cyanomethyl-5-methylbenzamide. The preparation method of this invention is simple, easy to operate, and involves a milder reaction, resulting in a high overall product yield. It is economical and environmentally friendly, and has high prospects for industrial production and commercial application.

The invention provides a preparation method of 3-cyanomethyl-5-methyl benzamide, and belongs to the technical field of medicine preparation.The preparation method comprises the steps that 5-methyl isophthalic acid serves as a raw material, 5-methyl isophthalic acid diester is prepared through a double-esterification reaction, then 3-hydroxymethyl-5-methyl benzoate is obtained through a selective reduction reaction, and the 3-cyanomethyl-5-methyl benzamide is obtained. The preparation method comprises the following steps: taking 3-hydroxymethyl-5-methylbenzoic acid as a raw material, carrying out hydrolysis to obtain 3-hydroxymethyl-5-methylbenzoic acid, then carrying out a hydroxymethyl substitution reaction, carrying out amidation to obtain 3-substituted methyl-5-methylbenzamide, and finally carrying out a cyanation reaction to obtain the target product 3-cyanomethyl-5-methylbenzamide. The preparation method disclosed by the invention is simple in process, easy to operate, milder in reaction and high in overall product yield, has the characteristics of economy and environmental protection, and has relatively high industrial production and commercial application prospects.

The invention discloses a synthetic method of 3-oxo-1-cyclobutane carboxylic acid, and belongs to the technical field of organic synthesis. The synthesis method comprises the following steps: S1, reacting chloroacetyl chloride with methyl acrylate in a solvent to generate 2, 2-dichloro-3-oxocyclobutane carboxylic acid methyl ester; s2, carrying out reductive dehalogenation on the 2-dichloro-3-oxocyclobutane carboxylic acid methyl ester, and converting the 2-dichloro-3-oxocyclobutane carboxylic acid methyl ester into 3-oxo-1-cyclobutane carboxylic acid methyl ester; and S3, carrying out a hydrolysis reaction on the 3-oxo-1-cyclobutane carboxylic acid methyl ester, so as to obtain the 3-oxo-1-cyclobutane carboxylic acid. The synthesis method of the 3-oxocyclobutane carboxylic acid is mild in reaction condition, high in yield and stable in product quality.

The present invention provides for a method for depolymerizing a lignin, said method comprising: (a) providing a metal catalyst, and (b) contacting a lignin to the metal catalyst, such that the metal catalyst depolymerizes at least a portion of the lignin into one or more lignin monomers.