58 results about "2-Chloroethanol" patented technology

During the preparation process, cellulose is dissolved completely in water solution with sodium hydroxide of 6 wt% and urea of 4 wt%, and is made to produce homogeneous hydroxyethylation with 2-chloroethanol in the water solution to produce water soluble hydroxyethyl cellulose. The cellulose has no obvious degradation during the reaction. The new process of preapring hydroxyethyl cellulose has low cost, no pollution, high product purity and good product homogeneity.

The invention provides an industrialized production and synthesis process of an adefovir dipivoxil raw medicine. The synthesis process comprises the following process routes of: reacting 2-chlorohydrin subjected to cholromethylation and triisopropyl phosphite to generate an adefovir lateral chain which is condensed and hydrolyzed with adenine to generate adefovir, and then carrying out condensation on the adefovir and chloromethyl pivalate to prepare the adefovir dipivoxil product. The invention has simple process, easy operation, safety, environment protection, mild reaction condition and high product purity, uses the most elementary raw materials and common reagents, and can be used for industrialized production. The invention is used for producing the adefovir dipivoxil raw material.

The invention provides a preparation method of a composite gas-sensitive material having high sensitivity, high selectivity and high stability and belongs to the field of functional materials. The invention mainly relates to a preparation method of a crystal-non-crystal metal oxide composite gas-sensitive material. The crystal-non-crystal metal oxide composite gas-sensitive material has high sensitivity to organic volatile compounds such as acetone, ethanol, 2-chloroethanol, chlorobenzene and formaldehyde, and has good heat stability and good selectivity. The preparation method has simple processes.

The invention discloses a synthetic method for 3-hydroxylmethal tetrahydrofuran. The synthetic method comprises the following steps: with 2-chloroethanol and diethyl malonate as raw materials, reacting under the action of alkaline in the presence of an organic solvent or in absence of a solvent to obtain an intermediate 2-ethoxy-diethyl succinate; then, reducing the intermediate 2-ethoxy-diethyl succinate by virtue of metal borohydride to obtain 2-hydroxymethyl-1,4-butanediol; and finally, producing 3-hydroxylmethal tetrahydrofuran under the action of a dehydrating agent. According to the synthetic method, the usage amount of the reducing agent metal borohydride is remarkably lowered, and yield of a byproduct sodium metaborate is reduced at the same time. The invention provides the synthetic method for the drug intermediate 3-hydroxylmethal tetrahydrofuran.

The invention discloses a synthesis method of 2,3-dihydrobenzofuran and belongs to the field of organic chemical synthesis. The preparation method comprises the steps that sodium phenate and 2-chloroethanol are used as raw materials, copper chloride and ferric chloride mixed solid is added as a catalyst, cooling is carried out after mixing, backflow and reflux reaction, an organic layer is collected, a sodium hydroxide solution is used for washing, 2-phenoxy ethanol is obtained, the 2-phenoxy ethanol is mixed with zinc chloride, manganous chloride is added as a catalyst, heating and reflux reaction are carried out, the sodium hydroxide solution is added for washing, reduced pressure distillation is carried out, fraction at the temperature of 88-90 DEG C is collected, and the 2,3-dihydrobenzofuran is obtained. According to the method, the copper chloride and ferric chloride mixture and the manganous chloride are used as the catalysts, the reaction technology and the reaction condition are optimized, the reaction temperature can be effectively decreased, reaction time can be shortened, the produced reaction by-products can be reduced, reaction efficiency can be improved, and the high economic benefit is obtained.

The invention discloses an ionic liquid segmented copolymer with an imidazole-contained main chain and a preparation method thereof. The preparation method comprises the following steps: under the protection of N2, causing imidazole to successively react with methyl acrylate and 2-chlorohydrin to generate a chlorination1-(3-methoxy-3-allyloxy)-3-(2-hydroxyl ethyl) imidazole ion liquid; carrying out condensation polymerization on the chlorination1-(3- methoxy-3-allyloxy)-3-(2-hydroxyl ethyl) imidazole ion liquid and 2,2,6,6-tetramethyl-4-bemidone-1-oxygen radical to obtain an imidazole ion liquid homopolymer of which the tail end contains an N-O free radical; and polymerizing the imidazole ion liquid homopolymer with styrene or the derivant thereof to obtain the ionic liquid segmented copolymer with an imidazole-contained main chain. The ionic liquid segmented copolymer is characterized in that the ionic liquid segmented copolymer with an imidazole-contained main chain is firstly prepared by a polycondensation method. The imidazole ion liquid with difunctionality is synthetized in advance; and condensation polymerization is carried out to obtain the ionic liquid homopolymer, wherein the tail end of the ionic liquid homopolymer contains the N-O free radical, and the main chain contains the imidazole. Then, the styrene or the derivant thereof is initiated by the N-O free radical to polymerize to obtain the ionic liquid segmented copolymer with an imidazole-contained main chain.

The invention provides a method for industrially producing adefovir. The method has a synthesis route that: 2-chloroethanol is subjected to cholromethylation and then reacted with triisopropyl phosphite to generate side chain of adefovir; and the side chain and adenine are subjected to condensation and hydrolysis to prepare the adefovir product. The method has the advantages of simple process, easy operation, safety, environmental protection, the most basic raw materials and common agents, mild reaction conditions, low cost, high purity of the product, and industrial production. The adefovir provided by the method can be used as a raw material medicament for producing adefovir dipivoxil.

The invention discloses a preparation method of a broccoli compound fertilizer with a characteristic of utilization rate improving. The preparation method comprises: uniformly mixing and stirring gum arabic and an ethanol solution, adding sodium hydroxide, carrying out heating stirring, adding 2-chloroethanol, stirring, adding maleic anhydride, continuously stirring, adjusting the pH value of the system to 6-6.8 with hydrochloric acid, adding starch, stirring, adding lauric acid, uniformly mixing, conveying into an extruder, extruding, heating, carrying out thermal insulation, and crushing to obtain a first preform; uniformly mixing corn cob powder, pine needle powder, coptis chinensis residue and an EM bacterial liquid, crushing, fermenting, carrying out high temperature sterilization, cooling, and carrying out air drying to obtain a second preform; and uniformly mixing potassium nitrate, calcium superphosphate, potassium dihydrogen phosphate, ammonium nitrate, magnesium humate, zinc humate, borax and iron humate, adding the first preform and the second preform, and uniformly stirring to obtain the broccoli compound fertilizer. According to the present invention, the broccoli compound fertilizer does not contain heavy metal pollutants, the preparation method is simple, and the obtained broccoli compound fertilizer meets the broccoli growth requirements.

The invention provides ionic liquid and a method for a homogeneous phase-modified reed-reinforced PE (polyethylene) composite material thereof, which belong to the field of synthesis and modification of materials. The ionic liquid is 1-vinyl-3-hydroxyethyl imidazole chlorine which is synthesized by N-vinyl imidazole and 2-chlorohydrin as raw materials according to the molar ratio of (1 to 1.5):1; the method adopts the ionic liquid, namely (1-vinyl-3-hydroxyethyl imidazole chlorine) to perform homogeneous phase modification on reeds, and the homogeneous phase-modified reed and PE are compounded, so that the homogeneous phase-modified reed-reinforced PE composite material is prepared. The ionic liquid designed by the invention can be used for effectively decreasing the surface polarity of the reeds, and increasing the dissolving capability of reed fibers. Compared with conventional methods, the method for performing homogeneous phase modification on the reeds by adopting the ionic liquid has the advantages of environment-friendly reaction solvents and recyclability; moreover, the homogeneous phase modification method improves the compatibility between the reeds and the PE, and the prepared homogeneous phase-modified reed-reinforced PE composite material has good mechanical property and excellent processability.

The invention relates to the technical field of chemical product preparation, and particularly relates to a synthetic method for alpha-acetyl-gamma-butyrolactone. The synthetic method comprises the steps of carrying out an aldol reaction on ketene dimer and 2-chloroethanol under the effect of a catalyst sodium alkoxide to obtain acetyl chloride ethanol acetate; preparing alpha-acetyl-gamma-butyrolactone: adding a solvent to acetyl chloride ethanol acetate, mixing with stirring, carrying out an intramolecular Claisen-Schmidt condensation reaction under the effect of an alkali catalyst, and directly generating alpha-acetyl-gamma-butyrolactone by cyclization. The synthetic method for alpha-acetyl-gamma-butyrolactone can prevent use of dangerous chemical products such as ethylene oxide, metallic sodium and the like and greatly reduce security risks. Besides, the synthetic yield is obviously higher than that of a conventional process, and production cost is significantly reduced.

The invention relates to a method for producing (meth)acryloyloxyethyltrimethylammonium chloride by transesterification, comprising two reactions: the first step, using (meth)acrylate and 2-chloroethanol as Raw materials, under the joint action of catalyst and polymerization inhibitor, while carrying out transesterification reaction, the small molecular alcohol is separated and evaporated through the packed tower, and the material at the bottom of the reaction kettle is subjected to vacuum distillation to obtain (meth)acrylic acid chlorohydrin ester. In the second step, (meth)chlorohydrin acrylate and trimethylamine aqueous solution react under normal pressure under the effect of a polymerization inhibitor and a basic anion exchange resin as a catalyst. After the reaction was completed, the water generated in the reaction process was separated by decompression, and then vacuum-dried at 80° C. to obtain the (meth)acryloyloxyethyltrimethylammonium chloride product, the content of which could reach more than 98%, and the total The rate can reach more than 90%. The invention has simple process, low production cost and mild reaction conditions, and is suitable for large-scale industrial production.

The invention discloses a headspace gas chromatography-mass spectrometry determination method of 2-chloroethanol in water. The headspace gas chromatography-mass spectrometry determination method comprises the following steps: 1), preparing a sample liquid: adding a water ample and sodium chloride into a headspace bottle, and sealing; 2), preparing a standard sample liquid: adding 2-chloroethanol with different concentrations and sodium chloride into headspace bottles, and sealing; 3), drawing a standard curve: analyzing the standard sample liquid prepared in the step 2) by headspace gas chromatography-mass spectrometry, and drawing the standard curve by using the concentration as an abscissa and the peak area as an ordinate; 4), detecting the sample liquid: analyzing the sample liquid by headspace gas chromatography-mass spectrometry to obtain the peak area, and substituting the peak area into a regression equation of the standard curve to obtain the concentration of the 2-chloroethanol in water. The determination method has the advantages of a large response value, a short detection time, good specificity, high sensitivity and the like.

The invention provides a synthesis method of 2-hydroxyl-3-chloropropyl-2'-chloroethyl ether, and an application thereof. The method comprises the steps of: firstly, mixing 2-chlorohydrin and a catalyst, and heating up to be at 45 DEG C; maintaining the temperature of 45 DEG C, and slowly dripping epoxy chloropropane into the mixture within 1-1.5 hours; then, controlling the reaction temperature to be within the range of 45-80 DEG C and the reaction time to be within the range of 3-5 hours, wherein the molar ratio between the 2-chlorohydrin and the epoxy chloropropane is 1.5-5.0, and the mass fraction of the catalyst accounts 0.2-1.5% of that of the epoxy chloropropane; and finally, carrying out vacuum distillation on reaction liquid, and collecting fraction under 1.33kPa at 114-117 DEG C. The 2-hydroxyl-3-chloropropyl-2'-chloroethyl ether synthesized by using the method can be taken as a comonomer for preparing polysulfide rubber, and the prepared polysulfide rubber has relatively good mechanical property and fuel resistance.

The invention discloses a synthetic method of ioversol. The synthetic method comprises the following steps: firstly, dissolving an ioversol intermediate 5-chloroacetamido-N,N'-bis(2,3-dihydroxypropyl)-2,4,6-triiodo-1,3-benzenedicarboxamide into a mixed solution of methanol, ethanol and barium hydroxide, and then adding 2-chloroethanol to carry out a nitrogen alkylation reaction to obtain a targetproduct ioversol; carrying out reduced pressure distillation on the obtained mixed solution to separate out the methanol, and separating out barium chloride by precipitation filtration according to the fact that the barium chloride generated after the nitrogen alkylation reaction is soluble in methanol and is insoluble in ethanol; and finally recrystallizing the solution containing the target product ioversol by using propylene glycol monomethyl ether to obtain the target product ioversol. According to the synthetic method disclosed by the invention, the quality and the yield of the synthesisof the ioversol are effectively improved, and the synthesis process is simplified.

The invention discloses a preparation method of alpha-(2,4-dichlorophenyl)-1h-imidazole-1-ethanol, and belongs to the technical field of organic synthesis. The method comprises the following steps that 1-(2,4-dichlorophenyl)-2-chloroethanol and imidazole are used as raw materials, hexafluoroisopropanol is used as a solvent, an inorganic carrier KOH / A12O3 is used as an alkaline catalyst, and through N-alkylation reaction, filtering, rotary evaporation, neutralization, filtering and recrystallization, the alpha-(2,4-dichlorophenyl)-1h-imidazole-1-ethanol is obtained. According to the preparationmethod of the alpha-(2,4-dichlorophenyl)-1h-imidazole-1-ethanol, reaction conditions are mild, reaction time is short, the solvent is easy to recover, the catalyst and the imidazole which does not participate in the reaction completely can be recycled, and the preparation method of the alpha-(2,4-dichlorophenyl)-1h-imidazole-1-ethanol is a green technology for synthesizing the alpha-(2,4-dichlorophenyl)-1h-imidazole-1-ethanol.

The invention provides a synthesis method of chloride 1, 3-bis (2-hydroxy ethyl) imidazole ionic liquid containing symmetry functional group, which compises mixing imidazole and 2-chloroethanol at the mol ratio of 1:2.1-1:2.2, adding anhydrous ethanol of 2-2.5 powered mol of the imidazole and metal sodium of 0.05-0.07 powered mol of the imidazole as catalyst, mixing and reacting for 7-8h at -1DEG C to 2DEG C, increasing temperature to 10-60DEG C, reacting for 40-48h, filtering to obtain light yellow liquid, depressurizing and evaporating out ethanol and unreacted 2-chloroethanol, washing via ethyl acetate, decolorizing via active carbon, filtering and passing through silicon gel column, standing at 0DEG C to -2DEG C, freezing for 40-48h and crystallizing to obtain pure 1, 3-bis (2-hydroxy ethyl) imidazole ionic liquid. Tests prove that the synthesized 1, 3-bis (2-hydroxy ethyl) imidazole ionic liquid has wide electrochemical window and active functional group, and the invention has wide application in the technical fields of conductive material and polyelectrolyte material.

The invention discloses a synthesis process of (2R)-(1,4-dioxane-2-yl)-N-methyl-methanamine hydrochloride. The synthesis process comprises the following steps: epoxy chloropropane and 2-chlorohydrin react to obtain (S)-3-(2-chlorooxethyl)-1-chloropropane-2-alcohol under the action of an salen catalyst; the (S)-3-(2-chlorooxethyl)-1-chloropropane-2-alcohol is subject to closed loop to obtain (2R)-2-[(2-chlorooxethyl) methyl]ethylene oxide under the action of carbonate; the (2R)-2-[(2-chlorooxethyl) methyl]ethylene oxide and hydroxide are subject to backflow reaction; toluenesulfonyl is added to the reaction product to obtain (2S)-1,4-dioxin-2-methyl-4-methyl p-toluenesulfonate ester; and the (2S)-1,4-dioxin-2-methyl-4-methyl p-toluenesulfonate ester and methylamine react in a high-pressure autoclave and hydrochloric acid is added to obtain the (2R)-(1,4-dioxane-2-methyl)-N-methyl-methanamine hydrochloride. In the synthesis process, a kinetic resolution technique is adopted so as to directly synthesize chiral compounds, raw materials can be obtained simply and easily, the reaction condition is mild, chiral separation is omitted, the cost is low and the synthesis process can be used for industrialized production.

The invention discloses a synthesis method of morpholine compounds, belonging to the field of organic synthesis. The invention aims to solve the problem of poor environment friendliness of the traditional synthesis method of morpholine compounds. The method comprises the steps of firstly, adding heterocyclic nitrogen compounds, persulfate and 2-chlorohydrin into a reaction vessel, and reacting at room temperature; secondly, adding a diluent, then, adding KOH, carrying out cyclization reaction at room temperature, next, filtering, and concentrating to be dry to obtain a solid; and thirdly, carrying out silica gel column chromatographic purification and separation on the solid obtained in the second step by taking a mixed solution composed of petroleum ether and ethyl acetate as an eluant to obtain the morpholine compounds. The synthesis method is capable of realizing reaction at normal temperature and normal temperature, mild in reaction condition, free of inert gas protection and simple in operation; and the persulfate serving as an oxidizing agent is cheap, easy to obtain, free of pollution, safe, environment-friendly and low in cost.

The invention discloses a preparation method of levo cloperastine fendizoate, which comprises the following steps: carrying out nucleophilic substitution reaction on 4-chlorobenzhydrol and 2-chloroethanol in a benzene organic solvent, so that an intermediate product is obtained; reacting the intermediate product with piperidine, so that racemic cloperastine is obtained; resolving the racemic cloperastine by using a resolving agent in a fatty alcohol solvent, so that levo cloperastine is obtained; and carrying out salt forming reaction on the levo cloperastine and a fendizoic acid, so that levo cloperastine fendizoate is obtained, wherein the resolving agent is an R-substituted dibenzoyl-L-tartaric acid, and R refers to alkyl, alkoxy, -Cl, -F, -Br or -H. In the method provided by the invention, in a fatty alcohol solvent, an R-substituted dibenzoyl-L-tartaric acid is adopted as a resolving agent for carrying out resolving on racemic cloperastine, and the resolving yield is high, so that the obtained levo cloperastine fendizoate has high optical purity, and has a high product yield.

The invention belongs to the technical field of a polyurethane material, and relates to flame retardant polyurethane hard foamed plastic. The flame retardant polyurethane hard foamed plastic is prepared from the following ingredients in parts by weight: 90 to 100 parts of mixed polyalcohol, 3 to 5 parts of foam stabilizers, 2 to 5 parts of antioxidants, 9 to 40 parts of flame retardants, 5 to 7 parts of chemical foaming agents, 5 to 7 parts of physical foaming agents, 1 to 2 parts of composite catalysts and 1.5 to 4.0 parts of isocyanate index, wherein the flame retardants include Al2(OH)3, dimethyl methylphosphate and 2-chloroethanol phosphate. The flame retardant polyurethane hard foamed plastic has the advantages that the flame retardant performance is obvious; through test, the OI (oxygen index) of the hard polyurethane foamed plastic reaches the standard that the OI is greater than B1 grade, specified in classification methods for combustion performance of building materials; theflame retardant polyurethane hard foamed plastic can be used at high temperature.

The invention discloses a synthetic method for 3-hydroxylmethal tetrahydrofuran. The synthetic method comprises the following steps: with 2-chloroethanol and diethyl malonate as raw materials, reacting under the action of alkaline in the presence of an organic solvent or in absence of a solvent to obtain an intermediate 2-ethoxy-diethyl succinate; then, reducing the intermediate 2-ethoxy-diethyl succinate by virtue of metal borohydride to obtain 2-hydroxymethyl-1,4-butanediol; and finally, producing 3-hydroxylmethal tetrahydrofuran under the action of a dehydrating agent. According to the synthetic method, the usage amount of the reducing agent metal borohydride is remarkably lowered, and yield of a byproduct sodium metaborate is reduced at the same time. The invention provides the synthetic method for the drug intermediate 3-hydroxylmethal tetrahydrofuran.

The invention discloses a p-aminophenyl-beta-hydroxyethyl sulfide preparation method comprising the steps that: (1) under the effect of a catalyst, sodium sulfide, sodium hydrosulfide and nitro chlorobenzene are mixed, such that nucleophilic substitution reaction, and nitro reduction reaction are carried out; and post-treatment is carried out, such that sodium p-aminothiophenol is obtained; (2) sodium p-aminothiophenol is subjected to a reaction with ethylene oxide, such that p-aminophenyl-beta-hydroxyethyl sulfide is obtained. According to the invention, a mixed solution of sodium sulfide and sodium hydrosulfide is used for replacing a polysulfide solution for carrying out the substitution and reduction reactions, such that the nucleophilic reagent SH<-> has high concentration at the beginning, and the substitution reaction can be smoothly carried out, side reaction can be inhibited, and yield can be improved. Ethylene oxide is used for replacing 2-chloroethanol in a condensation reaction with sodium p-aminothiophenol, such that production process is reduced, and production cost is reduced.

The present invention discloses (2í»-thiocyano) ethyl cinnamate compound with the chemical structure shown. The (2í»-thiocyano) ethyl cinnamate compound is prepared with cinnamic acid and 2-chloroethanol as material, and through esterification to obtain intermediate (2í»-chloro) ethyl cinnamate and the subsequent reaction of the intermediate to thiocyanate inside solvent. The preparation process is simple, low in cost and clean. The compound of the present invention contains thiocyanic radical with synergistic antiseptic and mildewproof effect and thus has antiseptic and mildewproof performance greatly higher than that of cinnamic acid and ethyl cinnamate and may be used as antiseptic and mildewproof agent in leather, timber, paint and papermaking industry.

The invention discloses a practical synthesis method for preparing an important medicine raw material 1-(2-hydroxyethyl)piperazine hydrochloride. In the presence of a proper solvent or in the absenceof a solvent, piperazine hydrochloride and 2-chloroethanol are stirred to react at 100-150 DEG C; 1-(2-hydroxyethyl)piperazine hydrochloride is directly obtained with high yield without protection ofone amino of piperazine.

A process for the complete destruction of gelled sulphur mustard (SM), comprising the steps of: (a) dissolving gelled sulphur mustard (SM) in organic solvent such as 2-chloroethanol, methanol, methyl cellosolve or mixtures of these to obtain a clear mixture, (b) incinerating the clear gelled sulphur mustard solvent mixture obtained from step (a); (c) dissolving residual gelled SM obtained from step (c) into non-toxic products; (d) chemically converting dissolved SM obtained from step (c) into non-toxic products.

The invention provides a process for the production of ethylene glycol from ethylene. An ethylene glycol stream comprises inorganic chloride contaminants and the process comprises steps of converting the inorganic chloride contaminants to 2-chloroethanol by reaction with ethylene oxide in one or more dehydration columns, and removing 2-chloroethanol in a waste water stream.

The invention belongs to the technical field of starch preparation, and particularly relates to a preparation method of special carboxymethyl hydroxyethyl starch for ham sausages. The preparation method comprises the following steps: (1) suspending; (2) carrying out alkalization treatment; (3) dropwise adding 2-chlorohydrin; (4) adding a methanol solution; (5) adding NaOH solid to carry out pretreatment; (6) adding chloroacetic acid at 50-65 DEG C and reacting for 4 hours; (7) carrying out neutral reaction; and (8) filtering, washing by using 80% methanol solution, and drying to obtain the carboxymethyl hydroxyethyl starch. The modified starch is mainly applied to ham sausages, so that the brightness and the stability of the ham sausages can be improved, and the anti-ageing target can be achieved.

The invention discloses a preparation method of 2-chloroethoxy-2-ethyoxylethanol. The preparation method comprises the steps: with 2-chloroethoxy and ethylene oxide as raw materials, performing a reaction in the presence of a catalyst to firstly obtain 2-ethyoxylethanol, removing the remaining solvent, namely a reactant 2-chlorohydrin, making the 2-ethyoxylethanol continuously react with the re-added ethylene oxide to obtain a target product 2-chloroethoxy-2-ethyoxylethanol. The preparation method has the advantages of being easy to operate during reaction, mild in system, less in side reactions, high in content and yield of products, and less in pollutants generated during the reaction.