131 results about "Ethyl bromoacetate" patented technology

Disclosed is a Sofalcone preparation method which mainly comprises, (1) subjecting p-hydroxybenzaldehyde and 2,4-ihydroxyacetophenone to condensation reaction under alkaline condition, obtaining 2,4,4-Trihydro-xychalcone, (2) subjecting 2,4,4-trihydro-xychalcone and 1-bromo-3-methyl-2-butene to condensation reaction, obtaining 2-hydroxyl-4,4-bis (3-methyl-2-butenyloxy) chalcone, (3) subjecting the 2-hydroxyl-4,4-bis (3-methyl-2-butenyloxy) chalcone and ethyl bromoacetate to condensation under the action of potasium carbonate, thus obtaining sofalcone. The mol ratio of p-hydroxybenzaldehyde, 2.4-dihydroxyacetophenone, 1-bromo-3-methyl-2-butene, and ethyl bromoacetate can be 1 : (0.90-1.50) : (1.60-2.55) : (0.60-1.25).

The invention discloses a quinazolinone compound containing 1, 2, 4-triazole thioether and synthesizing method and application of quinazolinone compound. The quinazolinone compound for preventing and curing plant pathogens is indicated by the general formula (I). Methyl anthranilate, formamide, ethyl bromoacetate, hydrazine hydrate, phenyl isothiocyanate, substitution benzyl halide or 2-chlorine-5 chloromethyl pyridine is used as raw material and subjected to six-step reaction to synthesize the target compound. The quinazolinone compounds A7, A8 and A19 are good in inhibitory activity on rice bacterial leaf blight germs. The quinazolinone compound A19 is good in inhibitory activity on citrus canker germs. The inhibitory activity on wheat scab germs of the quinazolinone compounds A14 and A18 and the inhibitory activity on apple rotting germs of the quinazolinone compound A8 are equal to that of control chemical hymexazol.

The invention discloses a PEG (Polyethylene Glycol)/mPEG (Methoxy Polyethylene Glycol) chemical modifier and a method thereof for preparing a water-soluble resveratrol prodrug. In the PEG/mPEG chemical modifier, PEG or mPEG is used as a vector, and the chemical modifier is prepared through reacting succinic anhydride, bromoacetate or isobutyl bromoacetate with amino acid. The preparation conditions and steps of the chemical modifier are simple. The chemical modifier is used for modifying the resveratrol to prepare the resveratrol prodrug, can change the water solubility and the stability of the resveratrol, is convenient to use and improves the bioactivity. When the prodrug is decomposed in vivo, amino acid required by the human body is also released while the resveratrol is released, thus the application scope of the prodrug is wider than that of the resveratrol.

The invention provides a hybridoma cell strain MOP1.0 capable of generating an anti-morphine monoclonal antibody, wherein the cell strain is preserved in China Center for Type Culture Collection with a preservation number of CCTCCNO. C2013159. The invention also provides the anti-morphine monoclonal antibody secreted by the hybridoma cell strain MOP1.0. The invention also provides a kit for detecting morphine in saliva. The invention further provides a detection method and a manufacturing method of the morphine detection kit. The hybridoma cell strain MOP1.0 has the benefit that the artificial antigen of obtained morphine keeps the structural specificity of morphine by utilizing ethyl bromoacetate as a cross-linking agent to activate the morphine. Through the adoption of a sandwich immune method, the using amount of antigens is effectively reduced, and the immunization time is shortened. The hybridoma cell strain MOP1.0 is high in secretion yield, and the anti-morphine monoclonal antibody obtained through secretion of the hybridoma cell strain MOP1.0 has the characteristics of high affinity, high specificity and high sensitivity. A detection product provided by the invention is more advantageous in the aspects of sensibility, specificity, detection limit and the like.

The invention discloses a preparation method of an alpha-glycosidase inhibitor 2,3,4-trihydroxy benzaldehyde-9'-O-berberine acylhydrazone, and can be used for preparing the medicines to treat diabetes. A structural formula of a compound is shown in the description. The preparation method comprises the following steps: 1) taking berberine hydrochloride as an initial raw material, demethylating under pressure reduction 190 DEG C condition, wherein the products can not be separated to obtain berberrubine (I), bridging the obtained compound I and alpha-ethyl bromoacetate through a nucleophilic substitution reaction to form a berberine ethyl acetate derivative (II); 2) performing hydrazinolysis of the compound II and hydrazine hydrate to obtain berberine hydrazides (III); and 3) performing nucleophilic addition-dehydration reaction on the compound III and the 2,3,4-trihydroxy benzaldehyde to obtain the 2,3,4-trihydroxy benzaldehyde-9'-O-berberine acylhydrazone (TM), and purifying the products through a recrystallization method. The 2,3,4-trihydroxy benzaldehyde-9'-O-berberine acylhydrazone has strong alpha-glucosidase inhibition activity through alpha-glucosidase inhibition experiment, and its inhibition performance is higher than that of a comparison product acarbose by 1.2 times.

The invention discloses a synthetic method of hydroxyl oximated calix[6]arene suitable for efficient uranium extraction. The synthetic method is completed by two steps: firstly, performing reaction between calix[6]arene and ethyl bromoacetate under the catalytic effect of anhydrous potassium carbonate to obtain a calix[6]arene ethyl acetate derivative; and secondly, performing reaction between the calix[6]arene ethyl acetate derivative and hydroxylamine hydrochloride under the catalytic effect of potassium hydroxide to obtain hydroxyl oximated calix[6]arene. The method is simple and convenient in synthetic line, mild in reaction condition and easy to control and realize; and synthesized hydroxyl oximated calix[6]arene has efficient extraction performance and selective complexation performance to uranium and has wide application prospect in uranium separation, uranium-bearing wastewater treatment and uranium recovery.

The invention discloses an imidazoline group-containing benzotriazole derivative, and a synthesis process and application thereof. The synthesis process comprises the following steps: taking benzotriazole as a raw material, and reacting with sodium monochloroacetate/ethyl chloroacetate/ethyl bromoacetate (wherein the reacting yield of the sodium monochloroacetate is highest) to form benzotriazole acetic acid, and performing dehydration and cyclization reaction with diethylenetriamine/triethylenetetramine/tetraethylenepentamine to generate the benzotriazole imidazoline derivative. The reaction conditions are easy to control; and the yield is high. The benzotriazole imidazoline derivative has a good corrosion inhibiting effect on YG8 hard alloy and Q235 low-carbon steel in an acidic water environment.

The invention discloses a 3, 5-dihydroxy-4-isopropyl diphenyl ethylene-ethyl bromoacetate-polyoxyethylene compound, namely polyoxyethylene-di(acetic acid-4-isopropyl-5-hydroxy diphenyl ethylene-3-phenolic ester). The original medicine is 3, 5-dihydroxy-4-isopropyl diphenyl ethylene (tolylene maud); and the modifier is polyoxyethylene and the linker arm is ethyl bromoacetate. The synthetic method of the compound includes three reactions, namely esterification reaction, hydrolysis reaction and esterification reaction. Compared with the original medicine, the compound has enhanced water-solubility and stability; the internal medicine distribution is changed; the bioavailability is enhanced; the synthetic method is simple; the reaction condition is mild; and the cost is low, without numerous unpleasant experimental procedures. In the method, the 3, 5-dihydroxy-4-isopropyl diphenyl ethylene-ethyl bromoacetate-polyoxyethylene compound can be easily made.

The invention provides a preparation method of an organic/layered double hydroxide (LDH) complex. The preparation method comprises the following steps of a) dissolving 1,10-dioxo-4,7,13, 16-tetranitro-18-crown-6 in a CH2Cl2 solvent, adding anhydrous potassium carbonate into the solution and mixing them, heating and refluxing the mixed solution, then adding ethyl bromoacetate into the mixed solution and refluxing it, then filtering and evaporating the refluxed solution to obtain an oil-like substance, adding hydrochloric acid solution into the oil-like substance, heating, refluxing and filtering the mixed solution, and evaporating the filtrate to make crystals be separated out to obtain 4,7,13,16-tetracarboxymethyl-1,10-dioxo-4,7,13, 16-tetraazaoctadecane (TECA), and b) mixing TECA, NaOH and methanamide, adding MgAl-NO3-LDH into the mixture, standing for 10 minutes to 16 hours, and then centrifuging, washing and drying the mixture to obtain a TECA/LDH complex, wherein a mass ratio of TECA to MgAl-NO3-LDH is 1. Through the preparation method, a TECA/LDH complex can be prepared in a short reaction time thus a production period of the TECA/LDH complex is saved; corrosive effects of methanamide on LDH laminates are reduced and compositions of the laminates are maintained well; and a crystallinity and a yield of complex products are improved.

The invention discloses a kind of coumarin-isatin type compounds, and a preparation method and a purpose thereof. The compounds possess a structure shown as a formula (I). The preparation method comprises taking 7-hydroxycoumarin and ethyl bromoacetate as raw materials to obtain [(2-oxo-2H-chromen-7-yl)oxy]acetic acid, and then performing hydrazinolysis reaction to obtain [(2-oxo-2H-chromen-7-yl)oxy]acetohydrazide, and finally reacting with various substituted isatins to obtain the corresponding target compounds. The compounds can be used as a raw material of an anti-diabetes medicament, and the preparation method is simple and easily-available in raw material and convenient to operate.

The invention provides a green synthesis method of ethyl bromodifluoroacetate. According to the method, 1,1-difluoro-1,2-dichloroethane is used as a starting material; elimination reaction is performed to obtain 1,1-difluoro-2-chloroethylene; the 1,1-difluoro-2-chloroethylene and bromine are subjected to addition to obtain 1,1-difluoro-1,2-dibromo-2-chloroethane; then, the elimination reaction is performed to obtain a 1,1-difluoro-2-bromine-2-chloroethylene; then, the 1,1-difluoro-2-bromine-2-chloroethylene and the bromine are subjected to addition to obtain 1,1-difluoro-1,2,2-tribromo-2-chloroethane; then, sulfur trioxide is used for oxidizing the 1,1-difluoro-1,2,2-tribromo-2-chloroethane; 1,1-difluoro-1-bromoacetyl chloride is obtained; finally, the 1,1-difluoro-1-bromoacetyl chloride and ethyl alcohol are esterified to obtain 2,2-difluoro-2-ethyl bromoacetate. The synthesis method has the advantages that the problems of recovery and utilization of waste materials of 1,1-difluoro-1,2-dichloroethane (R132b) are solved; no organic solvents are used in the reaction process; the oxidation step uses SO3 for oxidation; high temperature and high pressure or concentrated sulfuric acid is not needed; the safety is enhanced; the discharging of waste acid is reduced; the green production requirement is met; the product yield is relatively high; the green synthesis method is suitable for industrial production.

The invention relates to a method for synthesizing tert-butyl 6-oxo-8-oxa-2, 5-diazaspiro[3.5]nonane-2-carboxylate, and mainly solves a technical problem of absence of a method suitable for industrialsynthesis at present. The method provided by the invention comprises the following three steps: step one, firstly enabling a compound 1, paraformaldehyde and tetrabutylammonium fluoride added into asolvent N, N-dimethylformamide to be in reaction to obtain a compound 2; step two, enabling the compound 2, ethyl bromoacetate and cesium carbonate to be in reaction in acetone to obtain a compound 3;and step three, enabling the compound 3 and iron and ammonium chloride to be in reaction in ethanol and water to obtain a final compound 4, wherein a reaction formula is as shown in the Specification.

The invention discloses a preparation method and a bacteriostatic activity of plant pathogen prevention and treatment compounds quinazolinone compounds containing a 1,2,4-triazolethione Schiff base, and concretely relates to compounds represented by general formula (I), and a preparation method thereof. The quinazolinone target compounds containing the 1,2,4-triazolethione Schiff base are synthesized from methyl ortho-aminobenzoate, methanamide, ethyl bromoacetate, hydrazine hydrate, carbon disulfide, potassium hydroxide and aromatic aldehyde through the steps of ring closure, alkylation, hydrazinolysis, salt formation, ring closure and a Schiff base reaction. Compounds F11 and F19 have better Xanthomonas oryzae and Xanthomonas axonopodis pv. citri inhibition activity than a contrast medicate bismerthiazol under 200mg/mL or 100mg/mL; and the synthesized compounds have medium to excellent Sclerotinia scleotiorum inhibition activity, and compounds F4, F5, F6, F8, F9, F17 and F25 have broad-spectrum inhibition activity on six test fungi.

The invention provides a hybridoma cell line COC 2B1 which is capable of producing an anti-cocaine monoclonal antibody and preserved in CCTCC (China Center for Type Culture Collection) with the preservation number being NO.C201727. The invention further provides the anti-cocaine monoclonal antibody secreted by the hybridoma cell line COC 2B1, a kit for detecting cocaine in urine as well as a detection method and a production method of the cocaine detection kit. The invention has the following beneficial effects: ethyl bromoacetate as a crosslinking agent is used for activating cocaine, and anobtained cocaine artificial antigen keeps structural specificity of cocaine. A continuous immunization method is adopted, antigen dosage is saved effectively, immunization time is shortened, secretionyield of the hybridoma cell line COC 2B1 is high, and the cocaine monoclonal antibody secreted by the hybridoma cell line COC 2B1 has the characteristics of high affinity, high specificity and high sensitivity. The detection product has more advantages in aspects of sensitivity, specificity, detection limit and the like.

The invention relates to the technical field of medicine synthesis, in particular to a preparation method of cyano reductase and gabapentin. The method comprises the following steps: by taking sodium hydride as a catalyst, carrying out condensation reaction on cyclohexyl methyl cyanide and 2-ethyl bromoacetate to generate 2-cyano-2-cyclohexyl ethyl acetate; under an alkaline condition, carrying out hydrolysis reaction on 2-cyano-2-cyclohexyl ethyl acetate to obtain 2-cyano-2-cyclohexyl acetic acid; and converting the 2-cyano-2-cyclohexyl acetic acid into gabapentin under the action of the cyano reductase. Aiming at the defects (the problem of traditional chemical preparation of gabapentin) of a literature scheme, cyano reductase is introduced, and a route is systematically optimized, so that reaction steps are reduced, and meanwhile, reaction conditions are milder and more environment-friendly. According to the route, the overall yield of gabapentin can be remarkably increased, and meanwhile, the gabapentin better meets the requirements of current green production.

The invention provides a preparation method of an artificial antigen of ketamine. The preparation method comprises the following steps: (1) preparing and detecting a hapten, namely reacting the hapten containing carboxyl from ketamine hydrochloride and ethyl bromoacetate by virtue of dissociation, arm linkage and hydrolysis; (2) preparing and detecting the artificial antigen, namely combining the hapten with bovine gamma globulin (BGG) by virtue of a carbodiimide method so as to prepare the artificial antigen of the ketamine, namely ketamine-bovine gamma globulin. The prepared artificial antigen of the ketamine can be utilized for preparing corresponding ketamine antibodies by virtue of animal immunization and can be applied for researches of various ketamine immunoassay methods, and a convenient, rapid and accurate way is provided for the detection of the ketamine.

The invention provides a preparation method for a ketamine artificial antigen. The preparation method comprises the first step of hapten preparation and detection, wherein an ester group is introduced through reaction with ethyl bromoacetate, hydrolysis is carried out under the alkaline condition, and ketamine hapten containing carboxy groups is obtained; the second step of artificial antigen preparation and detection, wherein the ketamine hapten and bovine gamma globulin (BGG) are combined through a carbodiimide method to prepare the ketamine artificial antigen, namely, ketamine-BGG. The prepared ketamine artificial antigen can be used for animal immunization, a corresponding ketamine antibody is obtained, the preparation method can be used for studies of various kinds of ketamine immunoassays, and a more convenient, quicker and more accurate approach is provided for ketamine detection.

The invention discloses synthesis of 2-(1-benzylpiperidine)-2, 8-diazaspiro[4, 5]decane. Directed at the shortages of expensiveness, low reaction yield, and difficult purification in previous synthesis methods of 2-(1-benzylpiperidine)-2, 8-diazaspiro[4, 5]decane, the invention provides the following synthesis route of: taking piperidine-4 carboxylic acid ethyl ester as the raw material and conducting protection on it, then bringing the protected raw material into butt joint with ethyl bromoacetate, and carrying out ring closing with 1-benzylpiperidine-4-ammonia, performing deprotection, and implementing reduction with tetrahydro lithium aluminum, thus obtaining the 2-(1-benzylpiperidine)-2, 8-diazaspiro[4, 5]decane. According to the invention, the whole process is easy to operate, the product is easy to purify, and the raw material cost is greatly reduced.

The invention relates to the technical field of pharmaceutical chemistry and in particular relates to a chrysin amide derivative as well as a preparation method and medical application of the derivative. A structural formula of the chrysin amide derivative provided by the invention is shown as a formula I; a substituent group R in the compound is a series of acylamino. The chrysin amide derivativeprovided by the invention has the characteristics of good water solubility, stability and pharmacological activity; the preparation method of each chrysin amide derivative is the same and comprises the following steps: connecting 7th-site hydroxyl of chrysin with ethyl bromoacetate and then hydrolyzing; finally, carrying out amide condensation reaction on a series of amide compounds respectively,so as to obtain a series of chrysin amide derivatives. A pharmacodynamic screening experiment result shows that compared with the chrysin, the compound has better water solubility and better uric acid lowering and gout and inflammation resisting effects and is a compound which has a prospect of being developed into a novel anti-gout drug.

The invention belongs to the field of organic synthesis, and particularly relates to a synthesis method of imidazo[1,2-alpha]pyridyl-3-formic acid. The method comprises the following steps: reacting N,N-dimethylformamidodimethyl acetal with 2-aminopyridine at 40-100 DEG C for 2-8 hours to obtain an N,N-dimethyl-N'-2-pyridylformamidine intermediate, reacting the intermediate with ethyl bromoacetate at 50-160 DEG C, and recrystallizing to obtain a pure product; carrying out hydrolysis reaction on ethyl imidazo[1,2-alpha]pyridyl-3-formate in a certain solvent for 1-5 hours; and after the reaction finishes, neutralizing with hydrochloric acid, filtering, washing with water, and drying to directly obtain the imidazo[1,2-alpha]pyridyl-3-formic acid pure product. The method has the advantages of accessible reaction raw materials, reasonable price, mild reaction conditions and simple after-treatment, and is easy to operate and control; and the product has the advantages of stable quality and high purity.