115 results about "Grignard reaction" patented technology

The invention relates to the technical field of synthesis of metal organic complexes, in particular to a preparation method of a metal organic complex, and aims to solve the problems that the metal organic complex is tedious to prepare, low in yield, high in cost, incapable of meeting industrial production requirements and the like in the prior art. The preparation method of the metal organic complex comprises the following steps: carrying out Grignard reaction on a Grignard reagent and (dimethylamino) acetone to prepare a first product; wherein the Grignard reagent comprises R-MgX, R is selected from any one of C1-C2 alkyl groups, and X is selected from any one of chlorine, bromine and iodine; the general formula of the first product is as shown in the following formula (I): # imgabs0 # (I); carrying out a complexation reaction on the first product and a salt of a first metal M to prepare a metal organic complex; the general formula of the metal organic complex is as shown in the following formula (II): # imgabs1 # (II); m is selected from any one of copper and nickel.

The invention relates to a synthesis process of p-chlorophenylboronic acid, which comprises the following steps: by taking tetrahydrofuran as a solvent and p-dichlorobenzene as an initial raw material, firstly preparing p-chlorophenylmagnesium chloride through Grignard reaction, then reacting the p-chlorophenylmagnesium chloride with boric acid ester in a microchannel reactor to obtain a p-chlorophenylboronic acid ester crude product, and then hydrolyzing, layering and carrying out oil-phase azeotropic distillation to obtain the p-chlorophenylboronic acid ester. And finally, recrystallizing by adopting a mixed system of an alcohol solvent and a benzene solvent to obtain p-chlorophenylboronic acid with the content of 98% or above. The synthetic process of the p-chlorophenylboronic acid is mild in reaction condition, simple and convenient to operate, low in cost, high in safety, high in product content and very suitable for being applied to industrial large-scale production.

The invention relates to a preparation method of (R)-3-amino-1-oxa-8-azaspiro [4.5] decane-8-carboxylic acid tert-butyl ester, which comprises the following steps: carrying out Grignard reaction on N-BOC-4-piperidone and allyl magnesium halide to obtain an intermediate 1; carrying out substitution reaction on the intermediate 1 and 3-halogenated propylene to obtain an intermediate 2; performing olefin metathesis reaction on the intermediate 2 under the action of a Grubbs catalyst to obtain an intermediate 3; carrying out nitration reaction on the intermediate 3 and nitric acid to obtain an intermediate 4; carrying out hydrogenation reduction reaction on the intermediate 4 to obtain a racemic intermediate 5; and carrying out chiral resolution on the intermediate 5 by using a resolving agent to obtain a target product. The preparation method provided by the invention is short in process route and simple to operate, does not generate a large amount of waste water and waste gas, and can achieve higher total product yield and chemical and chiral purity.

The invention relates to the technical field of organic synthesis, in particular to a method for constructing Orforglipron tetrahydropyran ring chirality through enzyme catalysis, which comprises the following steps: step S1, taking SM1 as a raw material, and carrying out hydrolysis resolution in a solvent, a buffer salt system and enzyme catalysis to obtain a chiral pure intermediate INT-1; step S2; performing ring closing on the INT-1 through Grignard reaction to synthesize a lactone intermediate; s3, carrying out Diball-H reduction, quenching, dichloromethane extraction and anhydrous sodium sulfate drying on the INT-4, and then reducing the INT-4 by using triethyl silane to obtain an intermediate INT3; step S4, coupling the INT-3 in the presence of a catalyst and a ligand to obtain an intermediate INT-4; step S5, carrying out deprotection and salification on the INT-4 to obtain an intermediate INT5; s6, closing an indole ring from INT5 to obtain a compound of which the general formula is A; chirality is constructed through enzyme catalysis, isomer impurities do not need to be split and separated through SFC when the chirality is constructed, the loss is reduced, the yield is increased, and a target product is obtained with high chiral selectivity; meanwhile, the cost is relatively reduced, and the cost is saved.

The utility model relates to a reaction device for Grignard reaction, which comprises: a Grignard reagent batching kettle; a Grignard reactor, wherein the Grignard reactor comprises a reactor body, a second jacket formed on the outer wall of the reactor body, a second agitator rotatably mounted in the reactor body and extending to the outside thereof, a second motor mounted on the top of the reactor body and connected to the second agitator, a plurality of second feed ports opened on the top of the reactor body, and a second discharge valve mounted on the bottom of the reactor body; a feed delivery component, wherein the feed delivery component comprises a feed delivery pipe connecting the first discharge valve and any of the second feed ports, a first flow meter mounted on the feed delivery pipe, and a first regulating valve mounted on the feed delivery pipe and located downstream of the first flow meter. In this way, the problems of overheating (i.e., energy accumulation) and spraying that may exist when a single reactor is used can be avoided.

The present invention relates to the technical field of organic synthesis, and specifically relates to a method for constructing the chirality of a pyran ring in Orforglipron by means of enzymatic catalysis, the method comprising the following steps: step S1, by using SM1 and SM2 as starting materials, carrying out a reaction under the action of a palladium catalyst and a ligand to obtain INT-1; step S2, under the catalysis of Pd / C, subjecting INT-1 to double bond hydrogenation reduction to obtain INT-2; step S3, in the presence of a solvent, a buffer salt system and enzymatic catalysis, subjecting INT-2 to hydrolysis and resolution to obtain a chirally pure intermediate INT-3; step S4, subjecting INT-3 to a Grignard reaction for cyclization, so as to synthesize a lactone intermediate INT-4; and step S5, subjecting INT-4 to reduction by means of Dibal-H, quenching same, performing extraction with dichloromethane, drying same with anhydrous sodium sulfate, and then performing reduction by means of triethylsilane to obtain a compound of general formula A. In the present invention, the chirality is constructed by means of enzymatic catalysis without the need of SFC resolution for separating isomeric impurities during the construction of the chirality, thereby reducing losses and improving yield, obtaining the target product at high yield and high chiral selectivity, and further saving expenses and reducing costs.

The invention provides a preparation method and device of prothioconazole. The preparation method comprises the following steps: carrying out Grignard reaction on o-chlorobenzyl chloride and magnesium powder in a mixed solvent of toluene and 2-methyltetrahydrofuran; the method comprises the following steps: carrying out Grignard addition reaction on a Grignard reagent and 2-chloro-1-(1-chlorocyclopropyl) ethanone; the preparation method comprises the following steps: carrying out substitution reaction on 1-chloro-2-(1-chlorocyclopropyl)-3-(2-chlorphenyl) propanol and hydrazine hydrate in an alcohol solvent; the preparation method comprises the following steps: carrying out ring closing reaction on 2-(1-chlorocyclopropyl)-1-(2-chlorphenyl)-3-hydrazino-2-alcohol, a formaldehyde solution, a sodium thiocyanate solution and a sodium hydrogen sulfate solution; the preparation method comprises the following steps: carrying out oxidation reaction on 2-(2-chlorocyclopropyl)-3-(2-chlorphenyl)-2-hydroxypropyl)-1, 2, 4-triazolidine-3-thioketone, air and inorganic alkali, so as to obtain prothioconazole. The method can improve the efficiency of the oxidation reaction and the yield and purity of prothioconazole, and is more suitable for industrial production of prothioconazole.

The invention relates to the field of chemistry or medicinal chemistry, in particular to a synthesis method of isoxazoline anti-parasitic drug lotirasodium. The synthesis method comprises the following steps: firstly, synthesizing an intermediate 1 (1, 2, 3-trichloro-5-(1-trifluoromethyl-vinyl) benzene); then synthesizing an intermediate 2 (5-bromo-4-methyl-2-thiophenecarboxime); the preparation method comprises the following steps: carrying out a 1, 3 dipolar cycloaddition reaction on an intermediate 1 and an intermediate 2 in sequence to obtain an intermediate 3, carrying out a Grignard reaction to obtain racemic acid, and finally carrying out chemical resolution and amide condensation in sequence to obtain lotirasodium. According to the novel synthesis method of the isoxazoline anti-parasitic drug lotirazine, wittig reaction is adopted for the first time to obtain the intermediate 1, operation is simpler and more convenient, and reaction conditions are mild. Besides, the synthesis method of the intermediate 2 is improved, so that the reaction conditions are milder, the operation is simpler, the cost is greatly reduced on the basis of reported reaction conditions, and the method is suitable for industrialization.

The present invention discloses a preparation process of Grignard alcohol, which uses magnesium and methyl chloride as reaction raw materials, tetrahydrofuran as a solvent, and iodine crystals as an initiator. The Grignard reaction is carried out under nitrogen to generate a Grignard reagent, and then the Grignard reagent reacts with p-chlorobenzophenone by an addition reaction to generate Grignard alcohol. The magnesium includes pre-treated magnesium powder and magnesium strips. By simultaneously using magnesium powder and magnesium strips with specific mass ratios and size ratios and pre-treating them, the present invention can ensure the stable progress of the reaction and improve the reaction yield; in addition, by carrying out the treatment of removing water and peroxides from tetrahydrofuran, while ensuring the process safety, the yield of the Grignard alcohol product can be further improved.

This invention discloses a method for synthesizing a venetum intermediate, specifically as follows: Step 1: In an organic solvent, 2,4-difluorobenzoic acid and 5-hydroxy-7-azaindole undergo an etherification reaction under the action of an acid-binding agent. After the reaction, post-treatment yields 2-((1h-pyrrolo[2,3-b]pyridin-5-yl)oxy)-4-fluorobenzoic acid; Step 2: 2-((1h-pyrrolo[2,3-b]pyridin-5-yl)oxy)-4-fluorobenzoic acid reacts with 1-((2-(4-chlorophenyl)-4,4-dimethylcyclohexene-1-)methyl)piperazine in… An amination reaction occurs under the action of a base. After the reaction, post-treatment yields 2-(7-azaindole-5-oxy)-4-(4-((2-(4-chlorophenyl)-4,4-dimethylcyclohexene-1-)methyl)piperazine-1-)benzoic acid, i.e., Venetantora intermediate III. The synthetic process provided by this invention avoids Grignard reactions and subsequent hydrolysis reactions, shortens the operation steps, simplifies the synthetic process, and provides a simple and easy-to-operate synthetic process. The raw materials are inexpensive and readily available, while avoiding the use of highly toxic raw materials. The production process is green and environmentally friendly, and suitable for industrial production.

The invention relates to the technical field of organic synthesis, in particular to a rapid synthesis method of a polysubstituted pyrimidine carboxylic acid compound. The rapid synthesis method of the polysubstituted pyrimidine carboxylic acid compound comprises the following steps: by taking 4, 6-dichloro-5-methoxypyrimidine as a raw material and tetrahydrofuran as a solvent, carrying out Grignard reaction to prepare an intermediate I, then carrying out Suzuki reaction to obtain an intermediate II, carrying out saponification reaction on sodium hydroxide, and then reacting with hydroiodic acid to obtain the polysubstituted pyrimidine carboxylic acid derivative. According to the rapid synthesis method of the polysubstituted pyrimidine carboxylic acid compound, the reaction only needs four steps, the conditions are mild, the atom utilization rate is high, the route is safer and more environmentally friendly, industrial production is facilitated, and the polysubstituted pyrimidine carboxylic acid compound can be used as an important pharmaceutical and chemical building block to be conveniently used for subsequent derivatization.

The invention discloses a preparation method of 4-chloro-2-fluoro-3-methoxyphenylboronic acid and a preparation method of the 4-chloro-2-fluoro-3-methoxyphenylboronic acid. The specific implementation process comprises the following steps: by taking 1-bromo-4-chloro-2-fluoro-3-methoxybenzene as a raw material, carrying out Grignard reaction on magnesium chips and an initiator in an organic solvent to synthesize 4-chloro-2-fluoro-3-methoxyphenyl magnesium bromide; and the 4-chloro-2-fluoro-3-methoxyphenyl magnesium bromide and boric acid ester are synthesized into the 4-chloro-2-fluoro-3-methoxyphenylboronic acid, and then the 4-chloro-2-fluoro-3-methoxyphenyl magnesium bromide and boric acid ester are synthesized into the 4-chloro-2-fluoro-3-methoxyphenylboronic acid. The novel synthesis method of 4-chloro-2-fluoro-3-methoxyphenylboronic acid is designed, the total synthesis yield of the method ranges from 88% to 95%, compared with an existing synthesis route, the problems that a traditional route relates to an ultralow temperature condition and strong alkali, is low in safety and high in cost are solved, and the method has the advantages of being simple, environmentally friendly, safe, efficient and the like and is suitable for industrial production. Meanwhile, the method has a relatively good industrialization prospect.

The invention belongs to the technical field of drying equipment for Grignard reaction, and particularly relates to an automatic moisture drying system and method for benzenetetrasolvent in maltol production, and the system comprises a pre-drying storage tank, a first-stage drying storage tank, a first-stage circulating pump and a first-stage drying tower; the bottom of the before-drying storage tank is connected with an upper inlet of a first-stage drying storage tank through a pipeline, a bottom outlet of the first-stage drying storage tank is connected with a first-stage circulating pump, an outlet of the first-stage circulating pump is connected with an upper inlet of a first-stage drying tower, and an outlet of the first-stage drying tower is connected with the upper inlet of the first-stage drying storage tank; an outlet of the first-stage circulating pump is connected with an upper inlet of the second-stage drying storage tank, an outlet of the second-stage drying storage tank is connected with an inlet of the second-stage circulating pump, an outlet of the second-stage circulating pump is connected with an upper inlet of the second-stage drying tower, and a lower outlet of the second-stage drying tower is connected with an upper inlet of the second-stage drying storage tank. According to the invention, the benzene tetrasolvent is automatically dried in maltol production, and manual operation is not needed.

The invention relates to the technical field of medical and chemical medicines, in particular to a novel synthesis method of L (-)-threo-3-hydroxyaspartic acid hydrochloride. The preparation method comprises the following steps: by taking cheap and easily available D-phenylglycinol as an initial raw material, firstly protecting amino with Boc anhydride, then oxidizing to obtain N-BOC-D-phenylalanine aldehyde 3, then carrying out Grignard reaction on the N-BOC-D-phenylalanine aldehyde 3 and vinyl magnesium bromide at low temperature to obtain corresponding o-amino alcohol, then reacting the o-amino alcohol with 2, 2-dimethoxypropane at 0 DEG C under the catalytic action of p-toluenesulfonic acid, and finally obtaining the 2, 2-dimethoxypropane. The obtained compound 4 is subjected to Upjohn dihydroxylation reaction and sodium periodate oxidation to obtain corresponding aldehyde, and then the aldehyde is oxidized by potassium permanganate under a weak acidic condition to obtain corresponding carboxylic acid 5. Oxidizing a benzene ring by taking ruthenium trichloride as a catalyst and sodium periodate as a co-oxidant to obtain dicarboxylic acid; and finally, refluxing and deprotecting by using hydrochloric acid to obtain the L (-)-chloro-3-hydroxyaspartic acid hydrochloride.

The invention relates to the technical field of chemical synthesis, in particular to a tubular reactor capable of continuously producing Grignard reagents, which comprises an initiator, a Grignard reaction elbow, a discharge elbow and a discharge valve which are connected in sequence. The initiator comprises a feeding hole, a feeding pump, a gas guide pipe, an inert gas valve and a feeding pipe, and is used for injecting and mixing a halogenated hydrocarbon solution and an initiator; the Grignard reaction bent pipe comprises a material supplementing opening, a gas guide pipe and an inert gas valve and is used as a Grignard reaction area; the discharging bent pipe can prevent metal magnesium in the Grignard reactor from overflowing, and meanwhile, the discharging bent pipe is connected with a downstream reactor or Grignard reagent split charging equipment through the discharging valve, so that the generated Grignard reagent is discharged out of the tubular reactor. The tubular reactor has the beneficial effects that by using the tubular reactor provided by the invention, the Grignard reagent can be continuously produced in a mode of supplementing metal magnesium on line, the Grignard reaction risk is reduced, and the production process flow of the Grignard reagent is simplified.

The invention provides a novel method for preparing an intermediate compound of aromatic sesquiterpenes Commiphoranes C-D. The method comprises the following steps: substituting the ortho-position of a compound 1 with iodine through n-butyllithium and diiodoethane to obtain a compound 2; removing methoxyl by using boron tribromide to obtain a compound 3; performing nucleophilic substitution on 3-allyl bromide and potassium carbonate to synthesize a compound 4; carrying out Grignard reaction to obtain a compound 5; oxidizing into a compound 6 through a Dess-Martin oxidizing agent; finally, (CH3Si) 3SiH and triethyl boron are subjected to intramolecular free radical series cyclization, so that synthesis of an aromatic sesquiterpene Commiphoranes C-D intermediate compound is successfully completed, sufficient preparation is made for follow-up total synthesis of the natural product, key intramolecular free radical series cyclization has the capacity of efficiently constructing a polycyclic system, and the synthesis process is simple and convenient. According to the preparation method, the defects of expensive reagents, long 14-step linear synthesis route, low yield and the like in the existing synthesis route are overcome; the popularization potential is high.

The utility model provides continuous reaction equipment for preparing sartan biphenyl and belongs to the technical field of reaction equipment. Comprising a support frame; the Grignard reaction cabin is stably mounted on the supporting frame and is used for carrying out a preparation reaction of a Grignard reagent; the coupling reaction cabin is stably mounted on the support frame and is used for carrying out coupling reaction to generate the sartan biphenyl; and the cooling part is stably mounted on the supporting frame. Through cooperation of the Grignard reaction cabin, the coupling reaction cabin and the cooling part, the temperature requirement of the coupling reaction is met under the condition of not additionally arranging heating equipment, the energy consumption and the cost are reduced, and meanwhile through structural cooperation of a pressure relief opening formed in one side of the gas storage cabin, an internal sealing plug, a spring and a plurality of gas inlet channels, the pressure relief opening is formed in the other side of the gas storage cabin. And the pressure can be automatically relieved when the air pressure in the air storage bin is too high.

The invention provides a continuous production method and device of diphenyldimethoxysilane. The method comprises the following steps: 1) continuously adding a fresh first solvent, halogenated benzene, a fresh second solvent a and magnesium chips into a Grignard reactor at the same time, and carrying out Grignard reaction to generate a Grignard reagent; 2) continuously overflowing the Grignard reagent into a substitution reactor, and mixing the Grignard reagent with a continuously pumped fresh monomer and a fresh second solvent b for substitution reaction to obtain a substitution reaction solution; 3) filtering the substitution reaction liquid, and continuously rinsing the filter cake with a fresh second solvent c to obtain a wet filter cake, filtrate and rinsing liquid; 4) drying and dehumidifying the rinsed wet filter cake under reduced pressure to obtain a liquid-phase material flow and magnesium salt; (5) continuously feeding the filtrate and the rinsing liquid in the step (3) and the liquid-phase material in the step (4) into a solvent distillation system, and distilling to obtain a crude product, a circulating first solvent, a circulating monomer and a circulating second solvent; recycling the circulating first solvent, the circulating monomer and the circulating second solvent; and 6) product distillation.

The invention discloses a high-yield synthesis method of elxalidone, and relates to the technical field of drug synthesis. 1-chloro-2-(trifluoromethyl) benzene and 4-(methylsulfonyl) aniline are used as initial raw materials; according to the present invention, the isaprorenone is obtained through the Grignard reaction, the addition reaction, the bromination reaction, the condensation reaction, the substitution reaction, the cyclization reaction, the reduction reaction, the substitution reaction and the chiral resolution, and the synthesis method has advantages of low raw material cost, short route, high yield and the like, and can be used for the quantitative production of the isaprorenone.

The application discloses a synthesis method of flurbiprofen and an intermediate thereof. The intermediate of the flurbiprofen is 3-fluoro-4-biphenyl boronic pinacol ester, and the synthesis method comprises the following steps: step A: 2-fluoro-4-bromobiphenyl is subjected to a coupling reaction with bispinacolyl diboron under the action of an alkali and a metal catalyst to obtain 3-fluoro-4-biphenyl boronic pinacol ester. The synthesis method of the flurbiprofen comprises the following steps: step C: 3-fluoro-4-biphenyl boronic pinacol ester is subjected to a coupling reaction with sodium 2-bromopropionate under the action of an alkali and a metal catalyst, and then the obtained reaction product is acidified to obtain flurbiprofen. According to the application, 2-fluoro-4-bromobiphenyl is prepared into 3-fluoro-4-biphenyl boronic pinacol ester, and then the 3-fluoro-4-biphenyl boronic pinacol ester is subjected to a Suzuki coupling reaction with sodium 2-bromopropionate to prepare flurbiprofen, the method has less side reactions, and the molar yield is high, which is obviously higher than the yield in the literature of preparing flurbiprofen by means of Grignard reaction.

The application provides a preparation method of 2,4,6-trifluorobenzoic acid, which comprises the following steps: 1) subjecting 1,3,5-trifluorobenzene to a bromination reaction to obtain 2,4,6-trifluorobromobenzene; and 2) subjecting the 2,4,6-trifluorobromobenzene to a Grignard reaction to obtain 2,4,6-trifluorobenzoic acid. The method has the advantages of short flow, simple process, high molar yield and high purity of 2,4,6-trifluorobromobenzene, low cost of 2,4,6-trifluorobenzoic acid prepared by the method, and relatively environmentally-friendly and safe operation process, and is suitable for large-scale production.

The invention relates to a synthesis method of (4-chlorphenyl) (4-hydroxy-3, 5-dimethoxyphenyl) ketone, belongs to the field of organic chemical synthesis, and provides a method for solving the problems of high cost, low yield and more byproducts in the existing preparation method, and the method comprises the following steps: 1) reacting a compound shown as a formula I with an acyl chloride substance under the protection of nitrogen to obtain a compound II; 2) mixing the compound shown in the formula II with alkali, dropwise adding a Grignard reagent, and carrying out Grignard reaction to obtain a compound shown in a formula III; and 3) demethylating the compound in the formula III under the action of Lewis acid to obtain a compound in a formula IV. The technical scheme provided by the invention has the beneficial effects that the method for synthesizing (4-chlorphenyl) (4-hydroxy-3, 5-dimethoxyphenyl) ketone is novel in process route, the total yield is greater than 50%, and the method has the characteristics of short route, high chemical purity, easiness in production and the like.

The invention relates to a synthetic method of 2-diphenylmethyl pyrrolidine or an acid salt of 2-diphenylmethyl pyrrolidine. In order to solve the problems of easy ring opening and low yield in the prior art, the invention provides a synthetic method of 2-diphenylmethyl pyrrolidine or an acid salt thereof, which comprises the following steps: in the presence of an alkaline reagent, performing amidation and esterification reaction on a compound pyrrole-2-formic acid as shown in a formula II and ethyl chloroformate in an ROH solvent to obtain a compound as shown in a formula III; r in the ROH solvent is alkyl; performing Grignard reaction with phenyl magnesium bromide to obtain a compound as shown in a formula IV; carrying out reduction reaction on the compound shown in the formula IV under the catalytic action of trifluoroacetic acid and triethyl silane to obtain a compound shown in a formula V; and carrying out hydrolysis reaction on the compound in the formula V under an alkaline condition to obtain the compound 2-diphenylmethylpyrrolidine in the formula I or the acid salt thereof. According to the method, ring-opening impurities can be effectively avoided, the yield is increased to 95% or above, and the purity reaches 99% or above.

The invention discloses a preparation method of arfamarana, which belongs to the technical field of medicine, and comprises the following steps: step 1, taking Sm1 as an initial raw material, and carrying out amidation reaction on Sm1 and Sm2 to generate Int-1; step 2, carrying out aldol condensation reaction on the Int-1 and Sm3 to obtain Int-2; and step 3, carrying out cyclization reaction on the Int-2 and hydroxylamine hydrochloride to obtain the final product arfamparin. According to the invention, the reaction conditions are mild, the harsh process conditions (high-risk reagents, diazotization reaction operation and Grignard reaction operation) are avoided, and the use of complex Oldershaw rectification water removal equipment is also avoided. The method disclosed by the invention is short in synthesis step and high in yield, in terms of Sm1, the total molar yield is up to 67.37%, the product purity is 99% or above, and the maximum single impurity is 0.1% or below.

The utility model discloses a special reaction kettle for Grignard reaction, and relates to the field of fine chemical engineering. The reaction kettle special for the Grignard reaction comprises a reaction kettle body, a stirring assembly used for stirring a solution is installed in the reaction kettle body, and the reaction kettle further comprises a separation disc which is fixedly connected into the reaction kettle body and located below the stirring assembly; the hollow filter column is rotationally connected to the center position of the bottom of the separation disc through a fixing rod; according to the reaction kettle, the separation disc, the water spraying pipe, the hollow filter column, the blade plate group, the circulating pump, the liquid pumping pipe and the liquid conveying pipe are matched for use, so that when the reaction kettle is used for Grignard reaction, excessive magnesium chips can be intercepted in the reaction kettle and can be continuously used by a reaction solution in the next reaction; and the residual magnesium chips can be prevented from blocking filter holes of the filter assembly to influence the flow speed of the solution, so that the smoothness of discharging the solution out of the reaction kettle is effectively ensured.

The invention relates to a uniform feeding device of a Grignard reaction kettle, which comprises a feeding ring, a fixed ring and a rotating part, the fixed ring is arranged in the reaction kettle, the feeding ring is rotatably mounted on the fixed ring, the feeding ring is provided with a ring groove, the bottom of the feeding ring is provided with a plurality of feeding holes, and the fixed ring is provided with a feeding pipe connected with an external feeding pump. One end of the feeding pipe is communicated with the annular groove, a stirring assembly is arranged in the reaction kettle, and the rotating part is arranged in the reaction kettle and connected with the stirring assembly; before reaction, a base solution is added into the reaction kettle, the feeding pump feeds materials into the annular groove of the feeding ring through the feeding pipe, the materials are discharged through the feeding hole in the bottom of the feeding ring, meanwhile, the stirring assembly stirs the materials, and the rotating part drives the feeding ring to rotate and discharge the materials for dropwise adding reaction. And low yield caused by overhigh local reaction concentration is not easy to occur.

The utility model relates to a solvent recovery device for Grignard reaction. The solvent recovery device comprises a tank body, a water inlet is formed in the tank body, a filter plate is arranged in the tank body, a filter screen is installed on the filter plate, a cover plate is arranged at an opening in the top of the tank body, a lifting mechanism is arranged on the tank body, the cover plate is connected with the filter plate, and a blow-off pipe is arranged on the lower side of the tank body. A water outlet pipe and an oil outlet pipe are arranged on the side wall of the tank body; when the filter screen on the filter plate is used for a period of time and needs to be cleaned, the lifting mechanism drives the cover plate to further drive the filter plate to move, so that the filter screen on the filter plate can be cleaned, and the filter screen on the filter plate can be cleaned. The filter screen is detached from the filter plate at the opening of the tank body for replacement, the lifting mechanism sends the filter plate back into the tank body, and the device has the effect that the filter plate is convenient to detach and replace.

This invention discloses a method for preparing tetraenestrol, comprising the following steps: S1. Etherification reaction: In a solvent and in the presence of a catalyst, compound I is etherified with methanol to generate compound II, yielding a solution of compound II; S2. Grignard reaction: The solution of compound II obtained in S1 is reacted with a Grignard reagent to generate compound III, yielding a solution of compound III; S3. Hydrolysis reaction: In the presence of an acid, the solution of compound III obtained in S2 is hydrolyzed to generate compound IV, yielding a solution of compound IV; S4. Dehydrogenation reaction: In the presence of a dehydrogenation reagent, the solution of compound IV obtained in S3 is dehydrogenated to generate compound V, yielding tetraenestrol. This preparation route features simple reaction operation, high overall yield, and high product purity, reducing the overall production cost.

The application belongs to the technical field of liquid crystal materials, and relates to a trans-decahydronaphthalene indole liquid crystal compound and a preparation method thereof. The application provides a trans-decahydronaphthalene indole liquid crystal compound, which has a chemical structural formula as shown in formula (I). The preparation of the compound of formula (I) comprises the following steps: obtaining a compound of formula (III) from a compound of formula (II) through a Grignard reaction, oxidizing the compound of formula (III) to obtain a compound of formula (IV), and obtaining the compound of formula (I) from the compound of formula (IV) through a Fischer indole synthesis reaction. The preparation method is simple in operation, high in product yield and purity, and the prepared trans-decahydronaphthalene indole liquid crystal compound can be applied to special liquid crystal materials.

The application discloses a modified polysilane-polysiloxane body type crosslinking copolymer scintillator and a preparation method thereof. The crosslinking copolymer scintillator is a body type crosslinking structure formed by crosslinking of modified polymethylhydrosilane and polymethylphenylsiloxane. In the application, a scintillation group with 2-3 aromatic rings is introduced into a Si-Si main chain through a Grignard reaction, so that an original sigma conjugated system is expanded into a sigma-pi and sigma-pi conjugated system. Correspondingly, introduced pi electrons and lone pair electrons (n electrons) are converted into pi to sigma transition and pi to n to sigma transition, so that the energy gap width is changed, and the fluorescence emission spectrum of the polysilane becomes adjustable. After modification, the conjugated system is expanded, and the intermolecular electron transfer is improved, so that the fluorescence intensity and the quantum yield of the polysilane are improved. The fluorescence intensity of the modified scintillation group is 20-40 times higher than that of the unmodified polysilane-polysiloxane crosslinking copolymer.