232 results about "Acetoacetic acid" patented technology

The invention discloses a method for preparing butyrate clevidipine. The method comprises that 2, 3-dichlorobenzaldehyde, acetoacetate propionitrile ester and 3-amino-2-methyl crotonate are mixed and one-pot Hantzsch reaction is conducted, base catalyst is added to remove 2-cyanoethyl to obtain key intermediate, the key intermediate reacts with n-butyric acid chloromethyl ester to obtain butyrate clevidipine crude product, and the crude product is recrystallized to obtain high-purity butyrate clevidipine. Raw material 3-amino-2-methyl crotonate can be prepared by using low-price methyl acetoacetate. Raw material acetoacetate propionitrile ester can be prepared by using diketene. The synthesis of all raw materials requires no chromatographic separation for purification. The intermediate is synthesized through one-pot Hantzsch reaction, the reaction speed is fast, the condition is mild, the technological reliability is high and the purity of the intermediate is high. The conditions for the reaction of the key intermediate and the n-butyric acid chloromethyl ester can be easily controlled, the operation is simple and convenient, the cost is low, the post treatment requires no chromatographic separation for purification, the purity of the obtained butyrate clevidipine is above 99.5 percent and the mass production can be realized.

A thermosetting composition having:

• • I. a curable polyester resin containing beta-ketoacetate moieties without vinyl unsaturations; and
  • II. a phenolic resin having at least one methylol group.

The curable polyester resin can be made by reacting a polyester resin with a compound containing a beta-ketoacetate moiety that does not contain a vinyl unsaturation such as alkyl acetoacetate compounds or diketene compounds.

The curable polyester resin can be dispersed in water or dissolved in a solvent and is suitable for waterborne or solventborne coating compositions. Phenolic based crosslinking coating compositions that contain these curable polyester resins cure well with phenolic resin crosslinking compounds.

The invention relates to a preparing method for self-healing polysaccharide hydrogel. The preparing method comprises the steps that cellulose is added into ionic liquid to be dissolved, the mixture is then cooled to the room temperature, and a cellulose solution is obtained; the cellulose solution is heated and dripped with tert-butyl acetoacetate under the protection condition of introducing nitrogen, a reaction is carried out at the constant temperature, the solution is then cooled to the room temperature, purified and subjected to vacuum drying, and acetoacetic acid cellulose is obtained; under the room temperature, a chitosan solution is added into the acetoacetic acid cellulose solution, oscillated and mixed, and the self-healing polysaccharide hydrogel is obtained. The polysaccharide hydrogel prepared through the method has the self-healing performance, and has the pH responsiveness at the same time. The preparing method is simple in process, rich in raw material and suitable for modification of most polysaccharide derivatives; meanwhile, due to the good biocompatibility of cellulose and chitosan, the prepared polysaccharide hydrogel has good application prospects in the fields such as tissue engineering repair, medicine controlled release and biological bionics.

Disposable test strips and a wet chemistry method for measuring each of beta-hydroxybutyrate alone, combined beta-hydroxybutyrate and acetoacetate or total ketone bodies (i.e., beta-hydroxybutyrate, acetoacetate and acetone) in human bodily fluid samples, including but not limited to urine, saliva or sweat are described. The test strips need only be dipped in the sample and can be used by anyone in almost any milieu. Measurement can be made electrochemically, spectrophotometrically, fluorometrically or by comparision to a color standard. Combined acetoacetate and beta-hydroxybutyrate which account for 97-98% of total ketone bodies and may be measured in a cyclic reaction that occurs at pH about 7.0 to about 8.3 with beta-hydroxybutyrate dehydrogenase, (beta-HBD), nicotinamide adenine dinucleotide, a tetrazolium dye precursor and an electron mediator. Using this reaction, false positive results obtained from urine samples taken from patients on sulfhydryl drugs are avoided. beta-HBD from some sources was found to cause false negative results in samples (e.g. urine) containing high chloride content due to chloride inhibition of beta-HBD. Using a simple test for chloride inhibition, it was found that beta-HBD from Alcaligenes is not so inhibited. Using either beta-HBD that is not inhibited by chloride or using 10-20 times the normal concentration of this enzyme eliminates false negatives in samples having substantial chloride content, such as urine, both in the reaction described above and in other reactions disclosed for measuring each of beta-hydroxybutyrate alone, combined beta-hydroxybutyrate and acetoacetate and total ketone bodies, all of which reactions occur in the pH range of about 8.6 to about 9.5.

A liquid antiseptic and cleanser having improved long-term stability includes at least the following principal ingredients: deionized water; silver ion, polypectate, and ethylenediaminetetraaceticacid (EDTA). Presently preferred embodiments of the technology also include glycerine; 1,2-propanediol (a.k.a. propylene glycol); at least one surfactant from any of the families of alkylsulfates, sulfonates, alkanolamides, betaines, amine oxides, sarcosinates and sulfosuccinates; and a buffering compound sufficient to achieve a pH value within a range of 7.2 to 7.8.

The invention discloses a method for synthesizing sunitinib, which comprises the following steps that: tert-butyl acetoacetate and acetylacetic ester are taken as initial raw materials, and tetra-substituted pyrrole is obtained through a nitrosification reduction reaction; then 2,4-dimethyl pyrrole-3-formic acid is obtained through the hydrolysis and is amidated; then an aldehyde group is utilized on position 5 of pyrrole through a Vilsmeier-Hacck reaction; and finally the obtained product and 5-fluorooxindole react to obtain the sunitinib. The method has low cost and simple operation, and is favorable for industrial production.

The invention discloses a method for asymmetrically reducing a carbonyl compound by biocatalysis in a water/ion liquid biphasic system, which belongs to the biochemical engineering technical field. The method takes a selective strain producing carbonyl reductase as a starting strain, and prochiral ketone as a substrate to perform reducing preparation of corresponding chiral alcohol in the water/ion liquid biphasic system; the method comprises the following steps that: Aureobasidium pullulans CGMCC No.1244 is used to catalyze 4-chloro-acetoacetic acid ethyl ester to perform the asymmetrical reduction preparation of (S)-4-chloro-3-hydroxybutyric acid ethyl ester, and Saccharoinyces uvarum ATCC 26602 is used to catalyze 4,4,4-trifluoroacetoacetate to perform the asymmetrical reduction preparation of (R)-4, 4, 4-trilfluoro-3-hydroxybutyrate. The method shows the advantages of no toxicity, no smell, difficult volatilization, good biocompatibility, no environmental pollution, simple product separation, easy recovery, repeated use and so on, of ion liquid. At the same time, the method improves the transformation rate, the concentration and an enantiomeric excess value of a reaction product, and quickens the process of the reaction.

The invention relates to a method for preparing alumina aerogel. Firstly, methyl acetoacetate and polyvinyl alcohol are used as raw materials; concentrated sulfuric acid is used as a catalyst; throughester exchange reaction, acetoacetic acid groups are grafted on polyvinyl alcohol to prepare a macromolecule complexing agent; secondly, massive alumina aerogel with high density, high intensity, lowshrinkage rate, high porosity, high specific surface area and concentrated hole diameter distribution is obtained through preparation by using aluminium chloride hexahydrate as an inorganic phase precursor, using the macromolecule complexing agent as an additive, using deionized water as a solvent and using propylene oxide as a network gel inducting agent through the sol-gel process and the supercritical drying and roasting processes. The macromolecule complexing agent is added into the sol-gel process as a gel guiding agent and a dispersant, so that metal aluminum ion sol is uniformly dispersed in the solvent and is restrained by a macromolecule chain segment into a core; the primary particle aggregation mode is changed, so that the microstructure of the aerogel is changed. Meanwhile, the density and the intensity of the gel are enhanced.

A drier of acetacetic acid alkyl ester metal chelate paint and its production are disclosed. The procedure is carried out by reacting alkyl alcohol with diketene to obtain acetacetic acid alkyl ester chelant, and synthesizing the chelant with inorganic metal salt to obtain drier of acetacetic acid alkyl ester metal chelate. Its advantages include solid storage, light color, non-toxic, various raw material resources, simple process and more output.

The invention discloses a leifsonia xyli HSO904-based short chain dehydrogenase, and an encoding gene, a carrier, engineering bacteria and application thereof. A gene of the leifsonia xyli HSO904-based short chain dehydrogenase has more than 90% of homology of a nucleotide sequence shown in SEQ ID NO. 1. A colon bacillus BL21/pET28a (+)-SDR prepared by the recombination of the short chain dehydrogenase is used as an enzyme source, 3, 5-bis-trifluoro methyl acetophenone, trifluoromethyl acetophenone, 4-hydroxyl-2-butanone, acetoacetic ester, 4-chloro ethyl acetoacetate, acetoacetic acid tert-butyl acetate and the like are used as substrates to prepare corresponding chiral compounds such as (R)-3, 5-bis-trifluoromethyl phenethyl alcohol, trifluoromethyl benzaldehyde ethanol, 2-hydroxyl-butyl alcohol, 3-hydroxy ethyl butyrate, 4-chloro-3-hydroxy ethyl butyrate and 3-hydroxy butyric acid tert-butyl acetate through a catalytic asymmetric reduction reaction.

An alkaline earth metal salt of beta-diketo compound is produced using 1 mol of a powdery alkaline earth metal compound and 2.04 mol or more of an aliphatic beta-diketo compound. The reaction may be carried out while supplying both components to a reactor continuously or intermittently, or may be carried out by adding one component to the other continuously or intermittently. The highest temperature during the reaction may be at 50° C. or higher. The reaction mixture may be aged, and then dried at a temperature of at 100 to 180° C. in an atmosphere of an inert gas. The alkaline earth metal compound may be calcium hydroxide, magnesium hydroxide, or barium hydroxide. The aliphatic beta-diketo compound may be represented by the following formula, particularly an acetoacetic acid ester or acetylacetone.According to the production method as mentioned above, highly stable alkaline earth metal salts of beta-diketo compounds of high quality can be produced.

The invention discloses a preparation method for 5-benzyl-7(S)-t-butyloxycarborylamino-5-aza-spiro[2,4]heptane. The method comprises the following steps: reacting benzoylamide acetoacetate as a raw material with 1,2-dichloroethane to obtain 3-cyclopropyl benzoylamide acetoacetate, brominating 3-cyclopropyl benzoylamide acetoacetate by NBS (n-bromosuccinimide) to obtain 1-bromo-3-cyclopropyl benzoylamide acetoacetate, cyclizing under alkaline conditions to obtain 5-benzyl-5-aza-spiro[2,4]heptane-4,7-diketone, further reacting with hydroxylamine hydrochloride to form an oxime compound-4-oxo-5-benzyl-7-oximido-5-aza-spiro[2,4]heptane, reducing by NaBH4 and boron trifluoride diethyl etherate to obtain 5-benzyl-7-amino-5-aza-spiro[2,4]heptane, performing chiral resolution by a resolving agent-L-camphorsulfonic acid to obtain 5-benzyl-7(S)-amino-5-aza-spiro[2,4]heptane, and reacting with di-tert-butyl dicarbonate ester to obtain 5-benzyl-7(S)-t-butyloxycarborylamino-5-aza-spiro[2,4]heptane. According to the method, an intermediate body-carbonyl does not need protection, raw materials are easy to get, a process route is simple, and the method is suitable for industrial production.

The invention discloses a preparation method of eltrombopag olamine (Eltrombopag). The preparation method comprises the following steps: carrying out azo coupling reaction by using 3'-amino-2'-hydroxy-biphenyl-3-carboxylic acid (II) and acetoacetic acid alkyl ester to obtain (Z)-2-[3'-(2'-hydroxyl-3-hydroxy-biphenyl) hydrazono]-3-oxo acid alkyl ester (III); carrying out condensation cyclization reaction on an intermediate (III) and 3,4-dimethyl benzene hydrazine to prepare the eltrombopag olamine (I). The method is concise in process, available in raw material, economical and environmental friendly, and beneficial to achievement of industrialization, and economic and technological development of the eltrombopag olamine crude drug can be facilitated.

The invention provides a method for preparing cilnidipine used as a dihydropyridine calcium antagonist, which comprises the following steps: 2-(3-nitrobenzyl) acetoacetic acid 2-methoxyethyl acetate 4 and beta-amino crotonic acid cinnamic ester 5 react in an alcohol solvent to obtain a coarse product of cilnidipine 1, and the coarse product of the cilnidipine 1 is recrystallized to obtain the cilnidipine 1. The method has the advantages of short reaction period, simple and convenient after-treatment, simple synthetic route, moderate process condition, and the like and is suitable for industrial production.

The invention relates to an acrylate emulsion. Acetoacetoxy ethyl methacrylate is taken as a functional monomer, an acetoacetic acid group reacts with amine to generate enamine in the neutralizing stage of synthesis of the emulsion, enamine participates in later curing crosslinking, the shrinking percentage of the functional monomer is low, and internal stress during curing shrinking of a film is relieved. The surface of a polyester film is coated with the acrylate emulsion, permeation and spreading of a coating solution on a function coating are facilitated after high-temperature horizontal stretching and curing, the adhesion force between the function coating and the polyester film is high, and shedding is prevented. The optical polyester film with the surface coating can be used for the fields of a reflecting film, a hardening film, a window film and the like, and the film reprocessing demands are met.

The invention discloses a water-based acrylate pressure-sensitive adhesive and a preparation method thereof. The pressure-sensitive adhesive is prepared from the following raw materials in parts by weight: 0.5 to 5 parts of acrylic acid or methacrylic acid, 30 to 50 parts of acrylate monomer, 1 to 10 parts of crosslinking functional monomer, 0.1 to 1 part of initiator, 0.5 to 5 parts of emulsifier, 0.01 to 0.5 part of buffering agent, 0.05 to 3 parts of molecular weight regulator, 0.5 to 10 parts of tackifying resin, 0.5 to 5 parts of pH regulator, 45 to 60 parts of deionized water and 0.5 to 5 parts of water-based additive, wherein the cross-linking functional monomer is at least one of beta-carboxyethyl acrylate, diacetone acrylamide, glycidyl methacrylate, acetoacetic acid ethyl methacrylate, methacrylamide ethyl ethylene urea, ethylidene urea ethyoxyl methacrylate and trimethylolpropane trimethacrylate; and the emulsifier comprises an anionic emulsifier and a nonionic emulsifier, and the weight percentage of the anionic emulsifier in the emulsifier is at least 10%. The water-based acrylate pressure-sensitive adhesive has the advantages of high peel strength, high retention, high adhesion and wide use temperature range.

A waterborne acetoacetate-functionalized alkyd coating composition is disclosed which includes an acetoacetate-functionalized alkyd resin, at least one drier, and water. The acetoacetate-functionalized alkyd resin is the reaction product of (i) an alkyd resin, and (ii) an alkyl acetoacetate. Also disclosed is a method of preparing a waterborne acetoacetate-functionalized alkyd coating composition which includes the step of contacting an acetoacetate-functionalized alkyd resin with at least one drier in the presence of water.

The invention discloses a dustproof and bactericidal type aqueous coating material for glass doors. The dustproof and bactericidal type aqueous coating material is characterized by being prepared from the following raw materials in parts by weight: 34-38 parts of aqueous polyurethane resin, 28-34 parts of acrylic epoxy resin, 8-12 parts of modified styrene-acrylic emulsion, 0.4-0.8 part of polyvinyl alcohol, 1-3 parts of diethylene glycol monoethyl ether, 0.3-0.6 part of alcohol-amine dipyrophosphate acyloxy glycolate titanate, 0.2-0.5 part of polyether modified polyorganosiloxane, 0.2-0.4 part of cellaburate, 0.3-0.6 part of dioctyl sodium sulfosuccinate, 0.4-0.7 part of acetoacetoxy ethyl methacrylate, 0.6-1.2 parts of climbazole, 3-5 parts of ethylene glycol, 0.5-1.0 part of graphene, 1-2 parts of pigment and 10-15 parts of deionized water. According to the aqueous coating material disclosed by the invention, on the basis of high adhesion, water resistance and alcohol acid resistance, the modified styrene-acrylic emulsion is added, so that the bactericidal, dustproof and anti-electrostatic effects of the coating material are improved; added climbazole has spectrum sterilization property, so that the quality of the coating material is further improved; and the coating material disclosed by the invention is simple in operation and low in production cost, does not contain benzene solvents and heavy metals, is harmless to human bodies and environment, is environment-friendly and safe and is suitable for being popularized.

The invention discloses a preparation method for N-alkyl-2-methyl-5-formyl-3-pyrrole formate and application of N-alkyl2-methyl-5-formyl-3-pyrrole formate in cigarette flavoring. The preparation method comprises the following steps: with D-glucosamine hydrochloride as a raw material, reacting D-glucosamine hydrochloride with acetoacetic acid esters in an aqueous NaHCO3 solution so as to produce a 2-methyl-5-1',2',3',4'-tetrahydroxybutyl-3-pyrrole formate derivative; then preparing 2-methyl-5-formyl-3-pyrrole formate under the action of sodium periodate; and then reacting 2-methyl-5-formyl-3-pyrrole formate with halogenated hydrocarbon in the presence of tetrabutylammonium bromide and anhydrous potassium carbonate so as to obtain an N-alkyl-2-methyl-5-formyl-3-pyrrole formate derivative. The preparation method is simple; and after application of the prepared derivative in a cigarette, fragrance quality of the cigarette is improved, fragrance quantity is increased, fragrance becomes soft and fine, and remaining fragrance is comfortable.