33 results about "Chlorobenzoates" patented technology

The invention relates to a diamond resin honing stone for ultra-precisely machining a cylinder sleeve platform anilox roller and a preparation method thereof. The diamond resin honing stone comprises the following raw materials in percentages by weight: 20-30% of epoxy resin, 5-15% of polyurethane, 2-6% of W7 diamond micron powder, 35-45% of electrolytic copper powder, 5-15% of cerium oxide powder and 4-12% of isobutyl 3,5-diamino-p-chlorobenzoate as a solidifying agent. The preparation method comprises the following steps of: mixing the raw materials according to percentages by weight, pouring and forming to prepare the diamond resin honing stone for ultra-precisely machining the engine cylinder sleeve platform anilox roller. The engine cylinder sleeve platform anilox roller which is precisely honed by utilizing the diamond resin honing stone prepared by the preparation method disclosed by the invention has uniform deep grooves, the uniform width and distance and high platform precision, and an engine cylinder sleeve reaches EU III and IV emission standards.

The invention relates to a preparation method of 7-chloro-5-oxo-2,3,4,5-tetrahydro-1H-1-benzazepine, which is an important intermediate for preparing arginine vasopressin V2 receptor antagonist Tolvaptan. The preparation method comprises the following steps: with methyl 2-amido-5-chlorobenzoate and ethyl 4-bromobutyrate as starting raw materials, reacting at a low temperature under the effect of an acid binding agent to generate secondary amine first, then carrying out Dieckman condensation reaction at a raised temperature to generate an intermediate mixture III, and finally carrying out hydrolysis to obtain the target compound 7-chloro-5-oxo-2,3,4,5-tetrahydro-1H-1-benzazepine. Compared with the existing method, the method provided by the invention has the advantages that the reaction steps are reduced, the two-step reaction is simplified to one-step reaction through temperature control, so the operation is simple, the processing is convenient, the product purity is high, and the yield is also greatly improved, thus the production cost can be reduced, and the benefits are increased.

The invention relates to a method for preparing 7-chloro-5-oxo-2,3,4,5-tetrahydro-1H-1-benzazepine, which is an important intermediate for preparing arginine vasopressin V2 receptor antagonist Tolvaptan. The preparation method comprises the following steps: with methyl 2-amido-5-chlorobenzoate and ethyl 4-bromobutyrate as starting raw materials, reacting under the effect of an acid binding agent to generate secondary amine, and then carrying out Dieckman condensation and hydrolysis reaction to obtain the target compound 7-chloro-5-oxo-2,3,4,5-tetrahydro-1H-1-benzazepine. Compared with the existing method, the method provided by the invention has the advantages that the reaction steps are reduced, the operation is easy and simple, the product purity is high, and the yield is also greatly improved, thus the production cost can be reduced and the benefits are increased.

A synthetic method for 2-chlorobenzonitrile is disclosed and includes the following steps: performing a reaction on o-chlorobenzoic acid and ammonia to generate ammonium o-chlorobenzoate, high temperature dehydration is performed to produce 2-chlorobenzamide, and the high temperature dehydration is performed again to generate the 2-chlorobenzonitrile. In a production process, especially ultrasonicor microwave catalyzed high temperature dehydration is utilized to produce the 2-chlorobenzonitrile, the yield is up to 93%, and the purity of products can reach 97%. And the method has the characteristics of short process route, high reaction yield, good product purity, safe and clean whole reaction process, and easy environmentally friendly treatment. Production of waste water of the 2-chlorobenzonitrile can be effectively reduced, clean production of the 2-chlorobenzonitrile is achieved, unreacted raw material o-chlorobenzoic acid and intermediates can be recovered and then recycled and utilized, and the production cost can be significantly reduced. Moreover, the method can avoid the defects that traditional process equipment is complex, is high in operation requirements and is low inproduct yield, has the characteristics of less "three wastes" and less pollution, is another ideal way to achieve industrial production, and has strong market competitiveness.

The invention discloses a preparation method of O-diphenylphosphine benzoic acid. The preparation method comprises the following steps of: (1) carrying out cracking reaction on alkali metal and triphenylphosphine in an organic solvent to generate diphenylphosphine alkali metal salt and phenyl alkali metal salt; (2) slowly adding diisopropylamine, and enabling diisopropylamine to react with the phenyl alkali metal salt completely; (3) slowly adding O-chlorobenzol formate or O-bromobenzol formate, and enabling the diphenylphosphine alkali metal salt and the O-chlorobenzol formate or the O-bromobenzol formate to carry out coupling reaction and generate O-diphenylphosphino benzoate; (4) firstly hydrolyzing under the alkaline condition, obtaining O-diphenylphosphino sodium benzoate, acidizing and neutralizing under the acid condition, and obtaining the O-diphenylphosphine benzoic acid. The preparation method disclosed by the invention has the advantages that phenyllithium produced by cracking is completely reacted by adding the diisopropylamine, so that the generation of side reaction is effectively suppressed, and the reaction yield is greatly increased; since the triphenylphosphine is adopted as a reaction material, compared with the chlorodiphenylphosphine, the production cost is greatly reduced.

The present invention relates to a kind of bornyl benzoate, its chemical structure is shown in following formula (I), and chemical name is (+)-2-chlorobornyl benzoate. The synthetic method of bornyl benzoate of the present invention is that (+)-borneol, 1.04 times of borneol quality 2-chlorobenzoic acid, 0.067 times of borneol quality p-toluenesulfonic acid are added in toluene, at 110 It was obtained by reacting at ℃ for 6 hours. The (+)-2-chlorobornyl benzoate of the present invention has low toxicity and the effect of penetrating the blood-brain barrier, and can promote medicines to penetrate the blood-brain barrier.

The invention discloses a method for extracting para-chlorobenzoic acid from ketene wastewater, which comprises the following steps: oxidizing sodium para-chlorophenylmethoxide in wastewater to obtain sodium para-chlorobenzoate, stratifying to separate part of organic matters, neutralizing with hydrochloric acid, crystallizing out para-chlorobenzoic acid, purifying by dissolving organic impurities in the crude product into DMF (N,N-dimethylformamide) and methanol to obtain a refined para-chlorobenzoic acid product, and drying to obtain the product. The purity of the product is greater than 99%, which is higher than that of the para-chlorobenzoic acid in the market.

The invention relates to a preparation method for 3-amino-4-hexadecyl chlorobenzoate. The method comprises the following steps: adding 3-amino-4-chlorobenzoic acid and n-hexadecanol into a water-carrying agent, carrying out heating to 50 DEG C, maintaining a constant temperature for 0.5 to 1 h, then adding a catalyst namely p-toluenesulfonic acid, continuing heating to 140 to 170 DEG C, carrying out a reaction under a refluxing state for 6 to 12 h, and stopping heating; adding an organic solvent into a reaction solution obtained in the previous step, then carrying out cooling crystallization,washing and filtering, and drying a filter cake so as to obtain a crude product; collecting a filtrate; adding an organic solvent into the crude product, carrying out dissolving under heating, and carrying out cooling crystallization and filtering; and drying a filter cake so as to obtain a finished product namely the 3-amino-4-hexadecyl chlorobenzoate. The preparation method provided by the invention improves the utilization rate of raw materials, improves the yield of a product, reduces the treatment amount of an industrial filtrate, reduces the cost of industrial production and is more favorable for industrial production.

The invention discloses an herbicide containing tralkoxydim and a preparation method thereof. The herbicide comprises the following components (by weight): 10-20 parts of tralkoxydim, 15-30 parts of methyl 2-amino-3-chlorobenzoate, 5-15 parts of bensulfuron-methyl, 8-12 parts of 2,3-difluoro-5-chloropyridine, 10-20 parts of 2-chloro-4-diethylamine-6-isopropylamine-1,3,5-triazine, 10-14 parts of acetochlor emulsifiable concentrates, 10-20 parts of atrazine, 1-3 parts of an organic silicon defoamer, 5-15 parts of mefenacet, 20-30 parts of sodium hexametaphosphate, 5-15 parts of sodium nitrate, 10-20 parts of citric acid, 20-30 parts of methyl isopropyl ketone, 5-15 parts of cyhalofop-butyl, 7-10 parts of bispyribac-sodium, 5-15 parts of bentazone, and 1-3 parts of a pesticide adjuvant. The prepared herbicide has the advantages of high efficiency, low toxicity, low residue, low cost and good control effect on grassy and broadleaf weeds.

A preparation method of isobutyl 3,5-diamino-4-chlorobenzoate comprises the following basic steps: step 1, putting raw material ester compound, a solvent, a catalyst Raney nickel and a dehalogenation inhibitor into a high pressure reaction kettle at one time, sealing, and adopting 0.2-0.3 MPa of nitrogen gas and hydrogen gas for replacing gas in the high pressure reaction kettle for 3 times respectively; step 2, after completely sealing in the step 1, adding the hydrogen gas pressure to 3.0 MPa, increasing the temperature of the high pressure reaction kettle, carrying out a reaction, and timely replenishing the hydrogen gas pressure to ensure that the pressure in the high pressure reaction kettle in the reaction process is maintained at 3.0 MPa; step 3, adding hydrogen gas to maintain the pressure at 3.0 MPa in the step 2, carrying out a reaction for about 1.5-2 hours, finishing the reaction after the system absorbs hydrogen gas no longer, and overall cooling; step 4, after the step 3 is finished, recycling the catalyst Raney nickel; step 5, carrying out reduced pressure concentration of a filtrate to be viscous, putting into a refrigerator, and cooling and crystallizing at low temperature; and step 6, desolventizing the solvent alcohol and the dehalogenation inhibitor, recycling and reusing. The method is low in cost, safe and feasible.

The invention discloses a 2-chloro-benzoate compound which has a novel structure and is shown as the general formula (I), wherein R1 is selected from H or methyl, R2 is selected from H or methyl, and R3 is selected from C1-C6 alkyl or benzyl. When R1 is selected from H and R2 is selected from methyl, carbon atoms connected with R1 and R2 in the general formula are in an S or R structural type. Orthe invention provides a compound which contains different contents of S and R structural types. The compound which is shown as the general formula (I) has extraordinary weeding activity after seedling.

The invention discloses an environment-friendly waterproof architectural decorative coating which is composed of the following components in parts by weight: 30-45 parts of elastic emulsion, 1-3 parts of wetting agent, 1-2 parts of dispersant, 1-5 parts of polyether glycol, 25 parts of toluene diisocyanate, 2-5 parts of chlorobenzoate, 2-3 parts of white carbon black, 2 parts of kaolin, 2 parts of pigment, 3 parts of thickener and 9 parts of dispersant. The product has the advantages of small degradation degree, high stability and long service life; and all the production raw materials are environment-friendly, and thus, no waste water, waste gas, waste slag or pollution is generated in the production and construction process.

The invention discloses a universal herbicide for flowers. The universal herbicide comprises the following components by mass: 12-16 parts of oriental plane leaves, 14-16 parts of the leaves of Cinnamomum camphora, 18-24 parts of pine needle water, 8-14 parts of bamboo leaves, 9-13 parts of quicklime, 12-14 parts of bentazone, 3-6 parts of a dispersant, 4-8 parts of Sophora alopecuroide, 7-9 partsof methyl chlorobenzoate, 2-4 parts of bensulfuron-methyl, 3-5 parts of fulvic acid and 10-14 parts of a safener. Most raw materials of the herbicide of the invention are natural plants, and the universal herbicide is prepared by refining mutually-promoting-and-restricting components and the like of plants, so the universal herbicide is safe, has low toxicity, specially kills weeds, is free of harm to flowers and plants, and especially has obvious effect on flowers and trees like Zephyranthes candida and Ophiopogon japonicus and other are particularly effective.

The invention provides a method for synthesizing 2-methoxy-5-aminosulfonylmethyl benzoate by a one-step method. The method is characterized by adding 2-methoxy-5-methyl chlorobenzoate, sodium amino sulfonate, a solvent and a catalyst to a reaction device and controlling the temperature at 45-60 DEG C to react for 8-16 hours; adding activated carbon for decoloration after reaction is completed and removing activated carbon, the catalyst and a byproduct sodium chloride through filtration; carrying out vacuum concentration on the filtrate, thus obtaining 2-methoxy-5-aminosulfonylmethyl benzoate, wherein the mole ratio of 2-methoxy-5-methyl chlorobenzoate to sodium amino sulfonate is 1 to (1-1.1). The method for synthesizing 2-methoxy-5-aminosulfonylmethyl benzoate by the one-step method has the advantages that the original technological process is short; the yield is high; the quality is good; no three wastes polluting the environment are generated, so that the method is very environment-friendly and is suitable for large-scale industrial production.

The invention belongs to the technical field of organic synthesis, and provides a preparation method of alpha-configuration aroyl bromo-sugar. Beta-configuration (2R)-3, 5-bis(4-chlorobenzoate)-2-deoxy-2-fluoro-2-methyl-beta-D-erythro-furanpentose is used as a raw material, and is subjected to methylsulfonylation to prepare a mixture containing alpha-sulfonylated sugar and beta-sulfonylated sugar, the proportion of the beta-sulfonylated sugar is increased through transformation, the property of the obtained SN2 configuration inversion feed liquid obtained through SN2-configuration inversion under the action of lithium bromide is stable, the configuration of the alpha-configuration aroyl bromo-sugar is not converted any more, and the yield of the alpha-configuration aroyl bromo-sugar is improved. In addition, the preparation method provided by the invention is more suitable for industrial application.

The invention provides a method for synthesizing p-methoxybenzyl [3-(aminomethyl)-oxetane-3-yl]carbamate p-chlorobenzoate. The method comprises the following steps: a, preparing a compound 2 from a cyclic imido group substituted compound 1, wherein the cyclic imido group is any one of phthalimide, succimide and maleimide; b, carrying out an amination reaction on a primary amine and the compound 2to generate a compound 3; and c, reacting the compound 3 with 4-chlorobenzoic acid to obtain a compound 4. A reaction route is shown in the description. The synthesis method is friendly to the environment, and is suitable for large-scale industrial production.

The invention discloses a synthetic method of methyl 4-chlorobenzoate. The synthetic method comprises the following steps: mixing 1,4-dichlorobenzene with N,N-dimethylformamide or acetonitrile and tetraethylammonium iodide or tetraethylammonium bromide or tetraethylammonium chloride or tetraethylammonium tetraborate or tetrabutylammonium iodide or tetrabutylammonium bromide or tetrabutylammonium chloride to form electrolyte, introducing carbon dioxide into the electrolyte at the room temperature for 30 minutes, carrying out electrolysis by virtue of a constant current (carbon dioxide is continuously introduced during the electrolysis until the electrolysis is finished), and carrying out esterification and post-treatment, so as to obtain methyl 4-chlorobenzoate. The synthetic method has the beneficial effects that a reaction system is simple and easy to control; rice C1 resource CO2 is taken as one of the raw material and is cheap, easily available and low in cost, the environmental pollution is avoided, and a novel path is opened for the research of environment-friendly synthesis of methyl 4-chlorobenzoate; and the synthetic method presents excellent application prospects in the industries of chemical engineering and electrons and is a process route with high industrial synthesis values.