442 results about "Chloroacetyl chloride" patented technology

The invention relates to a fluorescence molecular probe for detecting zinc ions. The fluorescence molecular probe has the following chemical structure. The fluorescence molecular probe is prepared by the following steps: carrying out a reaction on 8-amino quinoline and chloroacetyl chloride under the effect of pyridine to obtain an intermediate; and carrying out a reaction on the intermediate obtained under the effect of KOH and KI to obtain the fluorescence molecular probe. Compared with other probes for detecting zinc ions, the probe is easier to be dissolved in water, good in selectivity, free from interference quenching of copper, cobalt and nickel ions and strong in infiltration capacity, and can be used for quickly detecting zinc ions in organisms and plants.

The invention discloses a preparation method of trifluoroacetic acid low in synthesis cost. The preparation method comprises the steps of (1) preparing 1,1-difluoro tetrachloroethane from 1,1-difluoroethane or chloride thereof through ultraviolet catalysis and a chlorine reaction; (2) implementing catalytic oxidation on the 1,1-difluoro tetrachloroethane to obtain 1,1-difluoro-1-chloroacetyl chloride, wherein in the catalytic oxidation, mol ratio of the 1,1-difluoro tetrachloroethane to an oxidizing agent is 1: (2-4), dosage of the catalyst is 0.5-5% of the total weight of an reactant, and reaction temperature is 50-70 DEG C; (3) carrying out hydrogen fluoride (HF) fluoridation on the 1,1-difluoro-1-chloroacetyl chloride under the catalyst to obtain trifluoroacetyl fluoride, wherein mol ratio of the 1,1-difluoro-1-chloroacetyl chloride to the HF is 1: (2-3), reaction temperature is 40-60 DEG C, and the catalyst is either antimony or antimony pentachloride; and (4) hydrolyzing the prepared trifluoroacetyl fluoride to obtain trifluoroacetic acid.

The invention relates to a synthesis method of an anticoagulant and a key intermediate, namely 3-morpholinone and 4-[(4-nitrophenyl)]-3- morpholinone, of the anticoagulant. The synthesis of intermediate uses aminoethanol and chloroacetyl chloride as starting materials. And the intermediate is obtained through condensation, transesterification, cyclization, recondensation and reduction reaction. The operation is simple and suitable for industrial production. Dichloromethane or triethylamine is used as a solvent in the synthesis process of the product. The product is obtained after simple post-treatment. The purity of HPLC (high performance liquid chromatography) is more than or equal to 99.5%. The process is simple and easy to operate, and is suitable for industrial production.

The invention discloses a surface imprinted polymer for catalyzing degradation of an organophosphorus pesticide and a preparation method thereof and relates to the field of surface imprinted polymers. The preparation method comprises the following steps of: preparing polystyrene seeds by a soap-free emulsion method; preparing polystyrene microspheres with particle diameter of 2 to 6 microns by a fractional swelling method; and bonding a chain transfer agent on the surfaces of the polystyrene microspheres. The preparation method comprises the main steps of: performing chloride acetylation on the microspheres with chloroacetic chloride, then aminating with ethydene diamine and then bonding the chain transfer agent with an amino; adding a template molecule under a proper solvent and performing graft polymerization on an amino acid derivative functional monomer and a cross-linking agent on the surfaces of the microspheres to form the needed polymer carrier surface template imprinted microspheres. The surface imprinted polymer with catalyzing, degrading and purifying functions on an organophosphorus compound is synthesized by taking an organophosphorus compound catalyzing and degradingreaction substrate as the template and organically combining the high-crosslinking degree insoluable porous polymeric microspheres with the template imprinting technology through a surface controllable graft hydrogel.

The invention discloses a ferroferric oxide nano-composite particle and a preparation method and applications thereof. The composite particle is a ferroferric oxide nano-composite particle with the particle size of 10-30nm, and 1,4-dihydroxy anthraquinone and fluorenylmethoxycarbonyl are modified on the surface of the ferroferric oxide nano-composite particle. The preparation method comprises the steps of: firstly, carrying out a hydrothermal method on ferric trichloride hexahydrate, sodium acetate, 1,6-hexanediamine and ethanediol to obtain the ferroferric oxide nano-composite particle, then producing 1,4-dihydroxy anthraquinone, chloroacetyl chloride, and N,N-dimethylformamide into dyes, then adding the ferroferric oxide nano-composite particle, sodium carbonate and the dyes into acetonitrile to carry out a reflux reaction, carrying out solid-liquid separation, washing and drying on the obtained reaction liquor to obtain an intermediate product, then dispersing the intermediate product into the N,N-dimethylformamide, adding dispersion liquid into the fluorenylmethoxycarbonyl, stirring for 2 hours, and carrying out solid-liquid separation, washing and drying to obtain a target product. The ferroferric oxide nano-composite particle can be used for fast detecting four heavy metal ions, namely copper, zinc, cadmium and mercury in an aqueous solution.

The invention relates to a preparation method of cefotetan. The method comprises the steps of: under an alkaline condition, reacting the starting raw material 7-MAC with chloroacetyl chloride in an organic solvent so as to obtain the intermediate CefoD-1; under nitrogen protection, adding aluminium trichloride into anisole, stirring for dissolving, and leaving the obtained solution for standby application; taking another organic solvent, into which the intermediate CefoD-1 is added under stirring, then adding the standby solution for reacting, thus obtaining the intermediate CefoD-2; reactingthe intermediate CefoD-2 with 3, 5-dithiol-4-isothiazole formic acid trisodium salt until that a sampled cefotetan tautomer is detected less than 4.0%, after the reaction conducting a post-treatment,thus obtaining cefotetan. With improved yield and reduced cost, the method of the invention, without final heating concentration, can generate products with a shallow color and almost invariant purity.

The invention relates to a preparation method of polyamino phosphoric acid functional-born polyether sulfone functional separating membrane. The preparation method mainly comprises the following steps: by taking trichloromethane, chloroacetyl chloride and anhydrous aluminum chloride as main reagents, performing chloracetylation to the polyether sulfone at room temperature; then by taking N,N-dimethylacetylamide as a solvent and tetraethylenepentamine as an amination reagent, performing amination to the polyether sulfone, subjected to chloracetylation, at the temperature of 80-85DEG C, and preparing chloroacetyl chloride-tetraethylenepentamine- polyether sulfone anion-exchange membrane; then in methanol and triethylamine solution, by taking paraformaldehyde and phosphorous acid as reagents, performing phosphorylation graft modification to the chloroacetyl chloride-tetraethylenepentamine- polyether sulfone anion-exchange membrane, to prepare the polyamino phosphoric acid functional-born polyether sulfone functional separating membrane. The preparation method has good technological stability, the chelated functional groups of the prepared polyether sulfone functional separating membrane are difficult to lose, and the heavy metal pollutants in water environment can be effectively removed.

The invention discloses a synthetic method for preparing roxatidine acetate hydrochloride with high purity. According to the invention, a starting material hydroxybenzaldehyde is subjected to condensation with piperidine to prepare 3-(1-piperidine methyl) phenol; an intermediate and 3-chloro amine hydrochloride are subjected to a backflow etherification reaction in a DMF at high temperature to obtain 3-(3-(1-piperidyl methyl) phenoxy) propylamine; the 3-(3-(1-piperidyl methyl) phenoxy) propylamine, chloroacetyl chloride and potassium acetate are subjected to a heating reflux reaction in a tetrahydrofuran solvent; and a HCl / THF solution is introduced to prepare a final product roxatidine acetate hydrochloride, with a total yield of 68%. The synthesis process has advantages of simpleness, low cost and high yield, can provide purity of the target product, and is in favor of industrial mass production of the product.

The invention relates to the field of the synthesis of chemical medicaments and discloses a preparation method of cefathiamidine; the method takes chloracetyl chloride as a raw material and comprises the following steps: (1) on the condition of the presence of a solvent, alkali is added so as to cause 7-ACA to be dissolved, and then the chloracetyl chloride is added for a condensation reaction; after the condensation reaction is finished, chloracetyl 7-ACA crystals are separated out with an acid; and (2) on the condition of the presence of both the solvent and a catalyst of a catalyzing amount, the chloracetyl 7-ACA reacts with N, N-di-isopropyl thiourea to produce the cefathiamidine. Besides the advantages of bromoacetyl-bromide preparation method of cefathiamidine, the technology of adopting chloracetyl chloride as the raw material to produce the cefathiamidine also has the advantages that: as no alkali is added into the reaction between the chloracetyl 7-ACA and the N, N-di-isopropyl thiourea, the produced cefathiamidine has lighter color, and better and more stable quality, is more beneficial to store and transport, improves the overall yield, lowers the cost and has broader prospects; and the price of the chloracetyl chloride is one sixth of that of the bromoacetyl bromide, which significantly reduce the cost.

The present invention belongs to the field of polymer compound material. The invention discloses an O-quaternary-N-thiourea chitosan, a preparation method and application thereof, and the chitosan is a chemical modified functional derivative of chitosan. The preparation method of the O-quaternary-N-thiourea chitosan comprises the following steps: adopting chitosan as a raw material and carrying out reaction with benzaldehyde to obtain chitosan Schiff base, then carrying out reaction with 2,3-glycidyl trimethyl ammonium chloride to obtain O-quaternary-N-chitosan Schiff base; carrying out deprotection of an amino group positioned on the second carbon atom (C2) of the O-quaternary-N-chitosan Schiff base through a methanol-hydrochloric acid solution to obtain O-quaternary chitosan, adding the O-quaternary chitosan to the mixture of ammonium thiocyanate and chloroacetyl chloride to carry out reaction, and then obtaining the O-quaternary-N-thiourea chitosan. The O-quaternary-N-thiourea chitosan provided in the invention achieves a substantial increase in antibacterial property compared with chitosan. The invention can be used in a plurality of application fields of antibacterial material, daily chemical products, industrial wastewater treatment and the like.

The invention provides a preparation method of propacetamol hydrochloride. The preparation method is characterized in that chloracetyl chloride and paracetamol carry out an acetylization chloride reaction in a polar aprotic solvent to obtain chloroactic acid-4-acetylamino phenyl ester which is directly aminated with diethylamine to obtain N, N'-diethylglycine 4-acetylamino phenyl ester, hydrochloric acid is used for adjusting the pH to be 4, and the propacetamol hydrochloride is obtained. The preparation method has the advantages of mild condition, convenient separation and purification, the total product yield is greatly increased, the use of the amount of the reaction solvent is low, and the preparation method reduces industrial pollution, and is applicable to industrialized production.

The invention discloses a preparation method of amino acid cationic liposome nanoparticles. The method comprises the following steps: (1) adding amino acid which is used as a raw material into lauric acid or normal alcohol acid so as to be subjected to esterification reaction, separating and purifying to obtain white solid or paste; (2) after the esterification reaction in the step (1) is finished, dropping chloroacetyl chloride in the obtained solid slowly to be subjected to chloroacetylation reaction, concentrating the reactant, then adding trimethylamine to be subjected to quaternization reaction, and performing the corresponding separation and purification to the obtained white or colorless solid; and (3) performing ultrasonic oscillation water dispersion on the solid obtained in the step (2) to obtain the corresponding amino acid cationic liposome nanoparticles. The method provided by the invention has low cost, is easy to operate, is suitable for most of amino acids and can be used for efficiently preparing amino acid cationic liposome nanoparticles with different structures.

The invention relates to a small-molecule fluorescent probe used for ratio recognition of human carbonic anhydrase, and a synthetic method and application thereof. The probe is prepared by reacting 4-amino-1,8-naphthalic anhydride with chloroacetyl chloride, diethylamine, 4-aminomethylbenzenesulfonamide and like. The synthetic method is simple to operate and uses cheap raw materials. The probe emits blue fluorescent light with a wavelength of ~470 nm in an aqueous solution and emits green to yellow fluorescent light with a wavelength of 525 to 560 nm in polar solvents like methanol, dimethyl sulfoxide, N,N-dimethyl formamide and ethanol. In a 20-mM phosphoric acid buffer, when human carbonic anhydrase 1 with an equivalent of 0 to 0.7 is gradually added, a fluorescence peak at a wavelength of ~470 nm gradually attenuates and a fluorescence peak at a wavelength of ~530 nm gradually intensifies. Thus, the probe provided by the invention can realize ratio recognition of human carbonic anhydrase and eliminates influence of external factors like equipment and samples.

The invention provides a method for preparing (2S)-N-chloracetyl-2-cyano-group pyrrolidine, which belongs to the technical field of chemical medicine midbody preparation methods. The preparation method comprises the steps: (1) L-proline and thionyl chloride generate acylation reaction to obtain L-proline chloride; (2) the L-proline chloride and ammonia water generate reaction to produce L-proline amide; (3) the L-proline amide and chloroacetyl chloride generate reaction to obtain (2S)-N-chloracetyl-2-carbamoyl pyrrole; and (4) (2S)-N-chloracetyl-2-carbamoyl pyrrolidine and phosphorus oxychloride generate dehydration reaction under low temperature condition to obtain the (2S)-N-chloracetyl-2-cyano-group pyrrolidine. The method has the advantages of saving material cost, being simple in technological process, moderate in reaction condition, low in operation difficulty, convenient in aftertreatment, stable in quality and suitable for mass industrial production, having operability, and improving yield of prepared products by a large margin.

The invention discloses a synthetic method of (S)-3-morpholinyl carboxylic acid, which comprises the following steps: (1) taking L-serine as a raw material to synthesize L-serine tert-butyl ester; (2) dissolving L-serine tert-butyl ester in dichloromethane, adding a dichloromethane solution of chloroacetyl chloride drop by drop to obtain N-chloroacetyl-L-serine tert-butyl ester; (3) dissolving N-chloroacetyl-L-serine tert-butyl ester in a toluene solution, adding the toluene solution of sodium ethoxide drop by drop to obtain (S)-5-oxo 3-morpholinyl carboxylic acid tert-butyl ester; (4) dissolving (S)-5-oxo 3-morpholinyl carboxylic acid tert-butyl ester in methanol, successively adding aluminum trichloride and sodium borohydride to carry out a reaction to obtain the (S)-3-morpholinyl carboxylic acid tert-butyl ester; (5) dissolving (S)-3-morpholinyl carboxylic acid tert-butyl ester in methanol, adding a methanol solution of hydrogen chloride for reacting to obtain the (S)-3-morpholinyl carboxylic acid. The method of the invention has the advantages of mild reaction condition, easily available raw material and less three waste, and is suitable for industrial production.

The invention belongs to the technical field of medicine and discloses diosgenin anti-tumor derivative and a synthesizing method thereof. The synthesizing method comprises the steps: after compound 3is obtained, utilizing triethylamine as alkali to react with chloroacetyl chloride to obtain 3-Csite amide compound 4; finally, reacting the compound 4 with nitrogen-containing compound to obtain a series of amide nitrogen-containing compound 5. The derivative disclosed by the invention and intermediates of the derivative wholly show high inhibitory activity and low cytotoxicity, the derivative 5aand 5e containing piperazine and the intermediate 4 show stronger inhibitory activity, and the derivative 5c, 5e, 5f, 5g, 5h and 5i shows low cytotoxicity to HBE cells. The results of the derivativedisclosed by the invention can provide certain reference value for structural modification of the diosgenin and analysis of anti-tumor activity of different radicals.

The invention discloses a preparation method for (R)- and (S)-alpha- alkoxy -beta-(1- imidazolyl)-2ú¼4-difluoroethylbenzenenitrate as optical-active imidazolyl aromatic derivant. Wherein, the synthesis method comprises: using chloracetyl chloride to acylate m-difluorobenzene into alpha- chloro-acetophenone; reducing ketone into alcohol; resolutioning racemic alcohol with organic-phase lipase catalyst to prepare (R)- and (S)- alcohol; on condition phase transferring, optical-active alcohol reacts with imidazole for N-alkylation reaction, then with benzylchlorine for O- alkylation reaction, using salt precipitation with nitric acid to obtain the objective product. The testings show: this product has antibacterial activity function, special the (R)- type, the technique has simple process and high yield.