11 results about "Chloranolol" patented technology

The invention discloses a preparation method of high-purity 2-fluoroethanol, and particularly relates to the technical field of preparation of 2-fluoroethanol, which comprises the following steps: S1, in a dual-catalyst system consisting of a phase transfer catalyst and a Lewis acid catalyst and an organic solvent, carrying out fluoridation reaction on 2-chloroethanol and anhydrous potassium fluoride at 60-120 DEG C for 2-10 hours to obtain 2-chloroethanol; and S2, sequentially carrying out integrated purification of filtration, reduced pressure distillation, adsorption treatment and rectification on the reaction mixture. According to the invention, through synergistic activation and mass transfer of double catalysts, the reaction rate and selectivity are significantly improved, the water segregator is utilized to remove reaction water to push equilibrium movement, the conversion rate is improved, and water and impurities are systematically removed by virtue of composite adsorption and precise rectification of molecular sieves and activated carbon, so that high-quality 2-fluoroethanol with high purity and low moisture is finally obtained. The whole preparation process is mild in condition, high in yield, good in safety and suitable for industrial production.

The invention belongs to the technical field of organic synthesis, and particularly relates to a production and preparation method of 2-chloroethoxyethanol. In the reaction process, chloroethanol is precooled to 0 DEG C, the temperature in the reaction kettle is controlled to be 3-8 DEG C, ethylene oxide is introduced in three stages, the pressure is kept to be 0.3-0.6 MPa, the temperature is low, and ethylene oxide is introduced in stages, so that the local concentration of ethylene oxide can be prevented from being too high, side reactions are reduced, and the reaction selectivity is improved. The used composite catalyst has sufficient active sites and is beneficial to diffusion of reactants and products, the supported phosphotungstic acid is used as a strong acid catalyst and can effectively activate epoxy bonds of ethylene oxide and promote nucleophilic addition reaction of ethylene oxide and chloroethanol, and the supported metal elements are capable of effectively activating the epoxy bonds of ethylene oxide and promoting the nucleophilic addition reaction of ethylene oxide and chloroethanol by adjusting the electronic properties of the catalyst. The catalytic activity and selectivity are improved, and the reaction is promoted together with phosphotungstic acid.

The invention relates to a preparation method of 1-chloroethyl cyclohexyl carbonate, and belongs to the technical field of synthesis of drug intermediates. In order to solve the problems of long route and high toxicity in the prior art, the invention provides a preparation method of 1-chloroethyl cyclohexyl carbonate, which comprises the following steps: mixing cyclohexanol and 1-chloroethanol under the action of organic alkali with a nitrogen-containing cyclic structure, and introducing carbon dioxide for reaction to obtain the 1-chloroethyl cyclohexyl carbonate. According to the method, high-toxicity phosgene does not need to be adopted as a raw material, the characteristic of one-pot reaction is achieved, the method further has the advantage of being short in reaction route, conversion loss of intermediate steps and loss of intermediate operation are better reduced, the obtained product has the effect of being high in product yield and quality, the yield reaches 98% or above, and the purity reaches 99% or above.

The invention relates to the technical field of fine chemical engineering, and particularly discloses a preparation method and a catalyst of 2-chloroethanol. Activated carbon provided by the invention has a high specific surface area and a porous structure, can be used as a mass transfer channel to promote diffusion of ethylene glycol and HCl to ZrO2 active sites, and can be used for preparing 2-chloroethanol through an addition reaction between double bonds. Maleic acid is grafted on the composite carrier, a carboxylic acid group passes through hydroxyl of protonated ethylene glycol to form a protonated intermediate, the nucleophilicity of the hydroxyl is reduced in the process, the electron deficiency of hydroxyl oxygen is enhanced, the hydroxyl oxygen is more easily substituted by Cl <->, and the catalytic effect of the catalyst is improved under the combined action of the carboxylic acid group and zirconium oxide; meanwhile, the activated carbon serves as a solid supporting body, so that the catalyst is easily recycled through filtration or centrifugation, the problem that a traditional homogeneous catalyst (such as adipic acid) is difficult to recycle is solved, and in addition, the catalyst provided by the invention still has a good catalytic effect after being recycled and reused.

The invention relates to a method for extracting spices containing ethylene oxide and 2-chloroethanol, and particularly relates to a method for extracting spices containing ethylene oxide and 2-chloroethanol, which comprises the following steps of: adding an inorganic salt solution into spices by using an acetonitrile solution as an extraction solvent to obtain two aqueous phases to promote the transfer of ethylene oxide and 2-chloroethanol to an organic phase. Meanwhile, the extraction efficiency of the compound is improved by utilizing a diluent swing effect generated by the eutectic solvent, and the efficient extraction of ethylene oxide and 2-chloroethanol in the spices is successfully realized.

The invention discloses a kind of preparation method of nicardipine hydrochloride, the preparation method is with 1,4-dihydro-2,6-dimethyl-4-(3-nitrophenyl) pyridine-3,5-dicarboxylic acid monomethyl ester and 2-chloroethanol as starting materials, obtains compound 3;Then react esterification with 2-naphthalenesulfonyl chloride, obtain compound 5;Replace with N-methylbenzylamine effect, then add hydrochloric acid to form salt, obtain crude compound 7;Finally, refine, obtain nicardipine hydrochloride. The present invention avoids using expensive condensing agents such as EDCI in preparation process for condensation, reduces production cost;And adopt specific mixed solvent acetone, tetrahydrofuran and acetonitrile in refining process, without using anhydrous magnesium sulfate drying, simplify preparation process, be beneficial to industrialized production. The content of prepared nicardipine hydrochloride is 99.98-100.10%, and benzene solvent is not detected, and does not contain potential genotoxic impurities, meets pharmacopoeia requirements.

The application relates to the technical field of organic synthesis, and particularly discloses a method for preparing 2-chloroethyloxy ethanol through combined catalysis, which comprises the following steps: under the catalysis of a main catalyst and an auxiliary catalyst, 2-chloroethanol and ethylene oxide are subjected to an alkylation reaction; after the alkylation reaction is completed, the alkylation reaction liquid is heated and desoluted to obtain a concentrated liquid, and 2-chloroethanol is recovered; and the concentrated liquid is distilled to obtain the target product 2-chloroethyloxy ethanol. The main catalyst and the auxiliary catalyst are combined to catalyze, the addition amount of boron trifluoride diethyl ether is greatly reduced, the generation amount of three wastes is reduced, the catalytic reaction rate is controllable, the side reaction is less, and the product has high purity.

The invention provides a preparation method of a diacylglycerol kinase inhibitor, which comprises the following steps: S1, reacting 4-fluorobenzyl bromide with magnesium under inert gas by taking iodine as an initiator to obtain a Grignard reagent B; s2, the Grignard reagent B and N-tert-butyloxycarbonyl-4-piperidone are subjected to an addition reaction, and an intermediate C is obtained through hydrolysis and deprotection; s3, carrying out Heck coupling reaction on the intermediate C, 4-fluorophenyl trifluoromethanesulfonate and a catalyst in the presence of alkali to obtain an intermediate D; s4, carrying out substitution reaction on the intermediate D and chloroethanol in the presence of alkali to obtain an intermediate E; s5, carrying out Mitsunobu reaction on the intermediate E to obtain an intermediate F; s6, carrying out addition reaction on the intermediate F and N, N '-thiocarbonyldiimidazole to obtain an intermediate G; and S7, carrying out cyclization reaction on the intermediate G, 2-methyl aminobenzoate and alkali to obtain the diacylglycerol kinase inhibitor R59949. The synthesis route disclosed for the first time has the characteristics of mild reaction conditions, reasonable design, cheap and easily available raw materials, high yield and the like, and provides theoretical support for biological evaluation and clinical application of R59949.

The invention relates to a directional transformation method for improving enzyme activity of halohydrin dehalogenase, and belongs to the technical field of bioengineering. According to a halohydrin dehalogenase mutant, single-point mutation or combined mutation is carried out on 60th alanine and 179th histidine in a sequence shown in SEQ ID NO.1 to obtain the mutant. Compared with wild halohydrin dehalogenase, the mutant obtained in the invention has obviously improved enzyme activity and dehalogenation efficiency in catalytic preparation of 1-chloro-2-propanol and 2-chloro-1-ethanol, the enzyme activity of the mutant is improved by 1.78 times, the dehalogenation efficiency is improved by 77.8%, and the mutant has a good industrial application prospect.

The utility model provides a 2-chloroethanol wastewater pretreatment device which comprises a pretreatment tank, a supporting block, a driving motor, a water inlet pipe, a water drainage pipe, a connecting pipe, a supportable turning and stirring spraying disc structure, a sprayable adding storage tank structure and a cleanable circulating auxiliary box structure, supporting blocks are respectively fixed at four corners of the bottom end of the pretreatment tank through bolts; a driving motor is fixed in the middle of the upper end of the pretreatment tank through a bolt. Through the arrangement of the rotating pipe, the H-shaped fixed pipe, the spraying disc, the water supply pipe, the adjusting pipe, the spraying head and the spiral plate, waste water can be turned in the rotating process of the spiral plate in the pretreatment process, water is supplied through the water supply pipe, then spraying is performed through the spraying head, the purpose of foam spraying elimination is achieved, and the waste water treatment efficiency is improved. Meanwhile, by adjusting a valve arranged in the middle of the upper end of the adjusting pipe, the pressure in the spraying process can be conveniently adjusted.

This application discloses a method for targeted modification to improve the activity of halohydrin dehalogenase, belonging to the field of bioengineering technology. The halohydrin dehalogenase mutant obtained by this application is produced by single-point mutation or combination mutation of alanine at position 60 and histidine at position 179 in the sequence shown in SEQ ID NO.1. Compared with the wild-type halohydrin dehalogenase, the mutant obtained in this application shows significantly improved enzyme activity and dehalogenation efficiency in the catalytic preparation of 1-chloro-2-propanol and 2-chloro-1-ethanol. The mutant enzyme activity is increased by 1.78 times, and the dehalogenation efficiency is increased by 77.8%, showing good prospects for industrial application.