CN112694425B - Method for preparing topramezone intermediate by using supergravity reaction - Google Patents
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Abstract
The invention discloses a method for preparing topramezone intermediate by using a supergravity reaction, which comprises the following steps: selecting a supergravity reaction, and adding 2, 3-dimethyl sulfide solution, hydrobromic acid and O3Gas enters the high-gravity reactor at a certain flow rate in proportion to be mixed with gas phase and liquid phase at a high speed, so that the insoluble hydrobromic acid and O3The gas is dispersed in the 2, 3-dimethyl sulfide solution to form a supersaturated solution of nano or micron-sized small bubbles, a solid-liquid-gas three-phase oxidation bromination one-pot reaction is carried out in a rotor containing a catalyst and a filler, and the reaction solution is subjected to desolventizing to obtain the high-purity 2, 3-dimethyl-4-methylsulfonyl bromobenzene. The method enables the oxidation bromination two-step reaction of the process to realize one-pot synthesis in the hypergravity reaction and obtain the topramezone intermediate with high yield and high purity. The method has the advantages of simple operation steps, environmental protection, small equipment volume, suitability for continuous industrial production, higher yield and content of final products and reduction of production cost.
Description
Technical Field
The invention relates to preparation of a fine chemical product intermediate, in particular to a method for preparing a topramezone intermediate by utilizing a supergravity reaction.
Background
Topramezone (topramezone), also called topramezone, is a novel high-selectivity benzyl ester pyrazolone herbicide, has the characteristics of high safety, excellent selectivity, broad-spectrum weed control activity, long aging, strong compatibility and the like, is higher than mesotrione and nicosulfuron in safety, is a corn field herbicide with the highest safety, and is also one of the herbicides with the lowest toxicity to mammals. The topramezone has a novel action mechanism, belongs to a p-hydroxyphenylpyruvate dioxygenase (HPPD) inhibitor, and has the advantage of good control effect on weeds resistant to glyphosate, triazine, ALS inhibitor and AC-Case inhibitor. The topramezone is mainly used for preventing and treating gramineous weeds and broadleaf weeds in corn fields, is mainly characterized by being safe to corn and afterculture crops, is a core factor of the product serving as a superior weeding product in the corn fields, and particularly can effectively prevent and kill resistant weeds such as green bristlegrass, crabgrass and eleusine indica which have poor control effect on the topramezone. The topramezone is applied to weeds such as crabgrass, cockspur grass, goosegrass herb, green bristlegrass herb, broomcorn millet, chenopodium album, polygonum, piemarker, redroot amaranth, ragweed, stramonium, cyathula chrysanthemum, purslane, xanthium sibiricum, black nightshade, tassel herb and the like. The topramezone has the advantages of high activity, extremely low dosage, wide post-emergence use suitable period, wide weed control spectrum, strong mixability, safety for corn and afterreap crops and the like, is mainly used for preventing and killing off annual warm-season gramineous weeds and broadleaf weeds in corn fields after emergence, can be compounded with atrazine or terbuthylazine, nicosulfuron, atrazine, mesotrione, clodinafop-propargyl, florasulam and the like, and the compounded product is also paid great attention. Topramezone CAS number: 210631-68-8 formula: C16H17N3O5S, molecular weight: 121.2.
2, 3-dimethyl-4-methylsulfonyl bromobenzene is an important intermediate of topramezone, and a general synthetic route is shown in figure 2. The literature is searched for the reaction of 2, 3-dimethyl sulfide with bromine to produce 2, 3-dimethyl-4-thiobromobenzene. After post-treatment, oxidizing the product with hydrogen peroxide to generate the target intermediate 2, 3-dimethyl-4-methylsulfonyl bromobenzene. The synthetic route is shown in figure 3. the two-step reaction has complex operation and lower yield. The combination of two normal operations with literature starting materials will yield the impurity monooxide rather than the target product intermediate. And the bromine is easy to cause damage to human bodies, does not meet the requirement of environmental protection and is not beneficial to industrial production. Therefore, there is an urgent need for improvement of the existing preparation method.
Disclosure of Invention
In order to solve the defects of low yield of two steps, complicated working section, complex post-treatment and the like in the prior art, the invention provides the method for preparing the topramezone intermediate by using the supergravity reaction, which has high yield, is green and environment-friendly and is suitable for continuous industrial production.
A method for preparing topramezone intermediate by using a supergravity reaction, comprising the following steps of:
s1: establishing a hypergravity reaction system
The hypergravity reaction system comprises a hypergravity reactor, a raw material pump, a raw material tank, a liquid circulating pump, a liquid storage tank and a liquid outlet pipe which are sequentially communicated;
the high-gravity reactor comprises a shell, a rotating body and a connecting pipe, wherein the rotating body comprises a rotating shaft and a cover body structure connected to one end of the rotating shaft; the bottom and the side wall of the cover body structure are provided with through holes; the connecting pipe is of a hollow structure, one end of the connecting pipe is fixedly connected with the connecting pipe, the packing layer is arranged at the hollow position of the cover body structure, the overlapped part of the packing layer and the cover body structure is arranged in the middle of the shell, and the connecting pipe and the packing layer are fixed when the rotating body rotates; the other end of the connecting pipe is communicated with one end of a three-way pipe, and the three-way pipe comprises a second gas inlet and a raw material feeding hole; the shell is also provided with a gas outlet and a first gas inlet;
s2: starting a hypergravity reaction
S21: mixing O with3After being measured by the rotameter, the gas enters the packing layer from the first gas inlet;
s22: the method comprises the steps that 2, 3-dimethyl sulfide solution stored in a raw material tank is metered by a raw material pump and then led into a raw material feeding hole, hydrobromic acid gas is metered by a rotor flow meter and led into a second gas inlet, the 2, 3-dimethyl sulfide solution and the hydrobromic acid gas meet at the communication position of a first gas inlet and the raw material feeding hole, the two gas and the hydrobromic acid gas are mixed and then pass through a connecting pipe, a plurality of small holes are formed in the connecting position of the connecting pipe and a packing layer, the raw material passes through the small holes, gas and liquid phases of the three raw materials are mixed at a high speed, and insoluble hydrobromic acid and O are enabled to be mixed3Dispersing the gas in the 2, 3-dimethyl sulfide solution to form a supersaturated solution of nano or micron-sized small bubbles;
s23: the supersaturated solution contacts with the catalyst in the packing layer under the action of supergravity, and O3Bromin generated by hydrobromic acid oxidation reacts with 2, 3-dimethyl thioether bromination to generate 2, 3-dimethyl-4-sulfur bromobenzene, and the 2, 3-dimethyl-4-sulfur bromobenzene is continuously reacted with excessive O under the action of catalyst in a packing layer3Oxidation reaction to produce 2, 3-dimethyl-4-methylsulfonyl bromobenzene and O2The reacted mixed gas is led out from a gas outlet, the reacted liquid leaves a packing layer due to the action of gravity and falls on the inner wall of a cover body structure, the cover body structure is driven by a rotating shaft to rotate, the reacted liquid is thrown onto the inner wall of a shell under the action of centrifugal force, the reacted liquid is converged to the bottom of the shell due to the action of gravity, the reacted liquid is led out from a liquid outlet pipe and enters a liquid storage tank, the reacted liquid is pumped to a raw material tank through a liquid circulating pump for recycling, and the reacted liquid is desolventized to obtain a topramezone intermediate 2, 3-dimethyl-4-methylsulfonyl bromobenzene.
Preferably, the solvent of the 2, 3-dimethyl sulfide solution is at least one or a mixture of more than two of glacial acetic acid, dichloroethane, dichloromethane, ethanol and acetonitrile, and the volume ratio of the 2, 3-dimethyl sulfide to the solvent is 1: 4-5.
Preferably, 2, 3-dimethylsulfide and O3The molar ratio is 1: 4.5-8.5.
Preferably, the molar ratio of the 2, 3-dimethyl sulfide to the hydrobromic acid is 1: 1.1-1.5.
Preferably, the catalyst is sodium tungstate dihydrate and is immobilized in the filler.
Preferably, the reaction temperature in the hypergravity reactor is 30 ℃ to 80 ℃.
Preferably, the internal reaction pressure of the hypergravity reactor is 0.5 MP-5 MP.
Preferably, the rotating speed of the rotating body is 300-1200 r/min.
Preferably, the filler layer (10) includes one or a mixture of two or more of silicon dioxide, titanium oxide, magnesium oxide, or carbon.
The invention has the beneficial effects that:
the effect is as follows: o is3Brominating and oxidizing hydrobromic acid gas and 2, 3-dimethyl sulfide in a hypergravity reactor under the action of a catalystThe preparation method by the pot method avoids the production of mono-oxide impurities by the conventional one-pot method, and improves the reaction rate and the final yield. The average yield is up to more than 95%.
The second effect is that: the single oxide impurities generated in the reaction in the preparation process of the 2, 3-dimethyl-4-methylsulfonyl bromobenzene can be greatly reduced by adopting the way of reaction and full mixing.
The effect is three: the supergravity mass transfer technology is adopted to replace the conventional reaction, thereby realizing the enhancement of the mass transfer process. In the hypergravity reaction, gas and liquid phases carry out mass transfer exchange in a great centrifugal force field generated by a rotor, a liquid film formed by the liquid is very thin under the action of centrifugal force, the surface is updated very fast, and the micro-element turbulence degree in the liquid is increased, so that the liquid phase mass transfer coefficient is greatly enhanced. In addition, the centrifugal force greatly improves the flooding limit of the equipment operation, so the volume mass transfer strength is improved by two orders of magnitude compared with the traditional equipment.
The effect is four: by using O3And hydrobromic acid gas to realize bromination oxidation, thereby improving the utilization rate of bromine atoms. The whole operation is simple and convenient, and continuous industrial production can be realized. And (5) making a table rate for the future green process serialization.
Drawings
In order to more clearly illustrate the technical solution in the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly described below. It is clear that the described figures are only some embodiments of the invention, not all embodiments, and that a person skilled in the art can also derive other designs and figures from them without inventive effort.
FIG. 1 is a block diagram of a high gravity reaction system of the present invention;
FIG. 2 is a schematic structural view of a rotating shaft of the present invention;
FIG. 3 is a chemical reaction scheme of a synthetic route for topramezone according to the present invention;
FIG. 4 shows the chemical reaction scheme for the conventional preparation of topramezone intermediate 2, 3-dimethyl-4-methanesulfonyl bromobenzene;
FIG. 5 shows the reaction scheme for preparing topramezone intermediate 2, 3-dimethyl-4-methanesulfonyl bromobenzene according to the present invention.
In the figure: 1-a first gas inlet, 2-a gas outlet, 3-a second gas inlet, 4-a raw material feeding hole, 5-a raw material pump, 6-a raw material tank, 7-a liquid circulating pump, 8-a liquid storage tank, 9-a liquid outlet pipe, 10-a packing layer, 11-a rotating shaft, 12-a shell, 13-a connecting pipe and 14-a cover body structure.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments. It is to be understood that these examples are for the purpose of illustrating the general principles, essential features and advantages of the present invention, and that the present invention is not limited by the following examples, and that the conditions employed in the examples may be further modified according to specific requirements, and that the conditions not specified are generally conditions in routine experimentation.
To demonstrate the necessity of selecting a hypergravity reaction, we made a routine control experiment.
Example 1 (control test)
2, 3-dimethylsulfide (10g, 0.065mol) and 50mL of 1, 2-dichloroethane were added to a 250mL three-necked flask, dissolved by conventional stirring, and cooled to 5 ℃. After the temperature was reduced, a 48% hydrobromic acid aqueous solution (14.4g, 0.08mol) and hydrogen peroxide (22.34g, 0.197mol) were added dropwise thereto at the same time, and the temperature was controlled to 5 ℃. After the dripping is finished, the temperature is kept for 10min, and the temperature is raised to 15 ℃ and kept for 2 h. And (3) detecting the reaction in a liquid phase. The peak area ratio of the 2, 3-dimethyl-4-methylsulfonyl bromobenzene product is 35.7 percent, and the peak area ratio of the single oxide impurity is 55.1 percent. The raw material was not detected.
The experiment proves that the bromination oxidation one-pot method of the 2, 3-dimethyl sulfide is difficult to realize under the conventional stirring instrument.
The following are examples of the reaction using supergravity
Example 2
Starting the hypergravity reaction of the silicon dioxide material, O3Gas is measured by a rotameter and is filled in the layer along the tangential direction by a first gas inlet 1 of the super-gravity reaction shell. A solution of 2, 3-dimethylsulfide in dichloroethane (50g of 2, 3-dimethylsulfide +250ml of dichloroethane) from a feed tank 6 is metered by a feed pump 5 and mixed with the feed from a second gas inlet 3 via a rotorHydrobromic acid gas metered by a flowmeter enters from a hypergravity reaction center together, gas and liquid phases are mixed at high speed, and 2, 3-dimethyl sulfide and O are controlled3And hydrobromic acid gas feed flow at a molar ratio of 1:6:1.3, the reaction temperature was set at 40 ℃ and the reaction pressure was 1 MP. The rotor speed is 800 r/min. Gas (containing O) after reaction2) The liquid is led out from the gas outlet 2, the liquid after reaction is thrown out of the packing layer, collected by the shell of the supergravity reaction and led out into the liquid storage tank 8 through the liquid outlet pipe 9 at the lower end of the supergravity reaction. And desolventizing the reaction solution to obtain 85.7g of topramezone intermediate 2, 3-dimethyl-4-methylsulfonyl bromobenzene. The purity of the product was determined by liquid chromatography to be 98.2% and the yield 97.4%.
Example 3
Starting the hypergravity reaction of the silicon dioxide material, O3Gas is measured by a rotameter and is filled in the layer along the tangential direction by a first gas inlet 1 of the super-gravity reaction shell. The dichloroethane solution (50g2, 3-dimethyl sulfide +250ml dichloroethane) of 2, 3-dimethyl sulfide from the raw material tank 6 is metered by the raw material pump 5 and enters the hypergravity reaction center together with the hydrobromic acid gas metered by the rotameter from the second gas inlet 3, the gas phase and the liquid phase are mixed at high speed, and the 2, 3-dimethyl sulfide, O and the like are controlled3And hydrobromic acid gas feed flow at a molar ratio of 1:5:1.3, the reaction temperature was set at 40 ℃ and the reaction pressure was 1 MP. The rotor speed is 800 r/min. Gas (containing O) after reaction2) The liquid is led out from the gas outlet 2, the liquid after reaction is thrown out of the packing layer, collected by the shell of the supergravity reaction and led out into the liquid storage tank 8 through the liquid outlet pipe 9 at the lower end of the supergravity reaction. The reaction solution is desolventized to obtain 85.87g of topramezone intermediate 2, 3-dimethyl-4-methylsulfonyl bromobenzene. The purity of the product was determined by liquid chromatography to be 96.3% and the yield 95.7%.
Example 4
Starting the hypergravity reaction of the silicon dioxide material, O3Gas is measured by a rotameter and is filled in the layer along the tangential direction by a first gas inlet 1 of the super-gravity reaction shell. Solution of 2, 3-dimethylsulfide from feed tank 6 in dichloroethane (50g of 2, 3-dimethylsulfide +250ml of dichloroethane)) The hydrogen bromide gas metered by the raw material pump 5 and the hydrobromic acid gas metered by the rotor flow meter from the second gas inlet 3 enter from the hypergravity reaction center, gas and liquid phases are mixed at high speed, and the 2, 3-dimethyl sulfide and O are controlled3And hydrobromic acid gas feed flow at a molar ratio of 1:6:1.5, the reaction temperature was set at 40 ℃ and the reaction pressure was 1 MP. The rotor speed is 800 r/min. Gas (containing O) after reaction2) The liquid is led out from the gas outlet 2, the liquid after reaction is thrown out of the packing layer, collected by the shell of the supergravity reaction and led out into the liquid storage tank 8 through the liquid outlet pipe 9 at the lower end of the supergravity reaction. And desolventizing the reaction solution to obtain 85.6g of topramezone intermediate 2, 3-dimethyl-4-methylsulfonyl bromobenzene. The purity of the product was determined by liquid chromatography to be 96.1% and the yield 95.2%.
Example 5
Starting the hypergravity reaction of the silicon dioxide material, O3Gas is measured by a rotameter and is filled in the layer along the tangential direction by a first gas inlet 1 of the super-gravity reaction shell. The dichloroethane solution (50g of 2, 3-dimethyl sulfide +250ml of dichloroethane) of 2, 3-dimethyl sulfide from the raw material tank 6 is metered by the raw material pump 5 and enters the hypergravity reaction center together with the hydrobromic acid gas metered by the rotameter from the second gas inlet 3, the gas phase and the liquid phase are mixed at high speed, and the 2, 3-dimethyl sulfide, O and the like are controlled3And hydrobromic acid gas feed flow at a molar ratio of 1:6:1.3, the reaction temperature was set at 60 ℃ and the reaction pressure was 1 MP. The rotor speed is 800 r/min. Gas (containing O) after reaction2) The liquid is led out from the gas outlet 2, the liquid after reaction is thrown out of the packing layer, collected by the shell of the supergravity reaction and led out into the liquid storage tank 8 through the liquid outlet pipe 9 at the lower end of the supergravity reaction. The reaction solution is desolventized to obtain 85.63g of topramezone intermediate 2, 3-dimethyl-4-methylsulfonyl bromobenzene. The purity of the product was determined by liquid chromatography to be 98.5% and the yield 97.6%.
Example 6
Starting the hypergravity reaction of the silicon dioxide material, O3Gas is measured by a rotameter and is filled in the layer along the tangential direction by a first gas inlet 1 of the super-gravity reaction shell. Of 2, 3-dimethylsulfide from a feed tank 6The dichloroethane solution (50g2, 3-dimethyl sulfide and 250ml dichloroethane) is metered by a raw material pump 5 and enters the high-gravity reaction center together with the hydrobromic acid gas metered by a rotor flow meter from a second gas inlet 3, the gas phase and the liquid phase are mixed at a high speed, and the 2, 3-dimethyl sulfide, the O and the like are controlled3And hydrobromic acid gas feed flow at a molar ratio of 1:6:1.3, reaction temperature set at 40 ℃ and reaction pressure 2 MP. The rotor speed is 800 r/min. Gas (containing O) after reaction2) The liquid is led out from the gas outlet 2, the liquid after reaction is thrown out of the packing layer, collected by the shell of the supergravity reaction and led out into the liquid storage tank 8 through the liquid outlet pipe 9 at the lower end of the supergravity reaction. The reaction solution is desolventized to obtain 85.62g of topramezone intermediate 2, 3-dimethyl-4-methylsulfonyl bromobenzene. The purity of the product was determined by liquid chromatography to be 98.6% and the yield 97.7%.
Example 7
Starting the hypergravity reaction of the silicon dioxide material, O3Gas is measured by a rotameter and is filled in the layer along the tangential direction by a first gas inlet 1 of the super-gravity reaction shell. The dichloroethane solution (50g of 2, 3-dimethyl sulfide +250ml of dichloroethane) of 2, 3-dimethyl sulfide from the raw material tank 6 is metered by the raw material pump 5 and enters the hypergravity reaction center together with the hydrobromic acid gas metered by the rotameter from the second gas inlet 3, the gas phase and the liquid phase are mixed at high speed, and the 2, 3-dimethyl sulfide, O and the like are controlled3And hydrobromic acid gas feed flow at a molar ratio of 1:6:1.3, the reaction temperature was set at 40 ℃ and the reaction pressure was 4 MP. The rotor speed is 800 r/min. Gas (containing O) after reaction2) The liquid is led out from the gas outlet 2, the liquid after reaction is thrown out of the packing layer, collected by the shell of the supergravity reaction and led out into the liquid storage tank 8 through the liquid outlet pipe 9 at the lower end of the supergravity reaction. And desolventizing the reaction solution to obtain 85.45g of topramezone intermediate 2, 3-dimethyl-4-methylsulfonyl bromobenzene. The purity of the product was determined by liquid chromatography to be 98.9% and the yield 97.7%.
TABLE 1
In table one, it can be seen that the molar ratio of the materials, the reaction temperature and the reaction pressure after the supergravity reaction are factors influencing the yield. The preparation yield of the brominated oxidation reaction by the one-pot method is more than 95 percent. And no mono-oxide impurities are generated. Achieves good experimental effect and realizes continuous production.
While the preferred embodiments of the present invention have been illustrated and described, it will be understood by those skilled in the art that the present invention is not limited to the details of the embodiments shown and described, but is capable of numerous equivalents and substitutions, all of which are within the scope of the claims appended hereto.
Claims (9)
1. A method for preparing topramezone intermediate by using a supergravity reaction is characterized by comprising the following steps of:
s1: establishing a hypergravity reaction system
The hypergravity reaction system comprises a hypergravity reactor, a raw material pump (5), a raw material tank (6), a liquid circulating pump (7), a liquid storage tank (8) and a liquid outlet pipe (9) which are communicated in sequence;
the high-gravity reactor comprises a shell (12), a rotating body and a connecting pipe (13), wherein the rotating body comprises a rotating shaft (11) and a cover body structure (14) connected to one end of the rotating shaft (11); the bottom and the side wall of the cover body structure (14) are provided with through holes; the connecting pipe (13) is of a hollow structure, one end of the connecting pipe (13) is fixedly connected with the connecting pipe, the packing layer (10) is placed in the hollow position of the cover body structure (14), the overlapped part of the packing layer (10) and the cover body structure (14) is placed in the middle of the shell (12), and the connecting pipe (13) and the packing layer (10) are fixed when the rotating body rotates; the other end of the connecting pipe (13) is communicated with one end of a three-way pipe, and the three-way pipe comprises a second gas inlet (3) and a raw material feeding hole (4); the shell (12) is also provided with a gas outlet (2) and a first gas inlet (1);
s2: starting a hypergravity reaction
S21: mixing O with3After being measured by a rotor flowmeter, the gas enters a packing layer (10) from a first gas inlet (1);
s22: 2, 3-dimethyl benzyl sulfide solution stored in a raw material tank (6) is metered by a raw material pump (5) and then is led into a raw material feeding hole (4), hydrobromic acid gas is metered by a rotor flow meter and then is led into a second gas inlet (3), the 2, 3-dimethyl benzyl sulfide solution and the hydrobromic acid gas meet at the communication position of the first gas inlet (1) and the raw material feeding hole (4), the two materials are mixed and then pass through a connecting pipe (13), a plurality of small holes are formed in the connecting position of the connecting pipe (13) and a packing layer (10), the raw materials enter the packing layer (10) through the small holes and meet with three raw materials, gas and liquid phases of the three raw materials are mixed at a high speed, and the difficultly soluble hydrobromic acid and O3Dispersing the gas in the 2, 3-dimethyl sulfide to form a supersaturated solution of nano or micron-sized small bubbles;
s23: the supersaturated solution is contacted with the catalyst in the packing layer (10) under the action of supergravity, O3Bromine generated by oxidizing hydrobromic acid and 2, 3-dimethyl methyl sulfide bromination reaction to generate 2, 3-dimethyl-4-sulfur bromobenzene, and the 2, 3-dimethyl-4-sulfur bromobenzene is continuously reacted with excessive O under the action of catalyst in a packing layer (10)3Oxidation reaction to produce 2, 3-dimethyl-4-methylsulfonyl bromobenzene and O2The reacted mixed gas is led out from the gas outlet (2), the reacted liquid leaves the packing layer due to the action of gravity and falls on the inner wall of the cover body structure (14), the cover body structure (14) rotates under the drive of the rotating shaft (11), the reacted liquid is thrown onto the inner wall of the shell (12) under the action of centrifugal force, the reacted liquid is converged at the bottom of the shell (12) due to the action of gravity, and then is led out from the liquid outlet pipe (9) to enter the liquid storage tank (8) and then is sent to the raw material tank for recycling through the liquid circulating pump (7), and the reacted liquid is desolventized to obtain the topramezone intermediate 2, 3-dimethyl-4-methylsulfonyl bromobenzene.
2. The method for preparing the topramezone intermediate by using the supergravity reaction according to claim 1, wherein the solvent of the 2, 3-dimethyl benzyl sulfide solution is at least one or a mixture of more than two of glacial acetic acid, dichloroethane, dichloromethane, ethanol and acetonitrile, and the volume ratio of the 2, 3-dimethyl benzyl sulfide to the solvent is 1: 4-5.
3. The process for preparing topramezone intermediate by using the supergravity reaction of claim 1, wherein the 2, 3-dimethyl methyl phenyl sulfide and the O3The molar ratio is 1: 4.5-8.5.
4. The method for preparing the topramezone intermediate by using the supergravity reaction, according to claim 1, wherein the molar ratio of the 2, 3-dimethyl methyl sulfide to the hydrobromic acid is 1: 1.1-1.5.
5. The method for preparing topramezone intermediate by using the supergravity reaction according to claim 1, wherein the catalyst is sodium tungstate dihydrate and is immobilized in a filler.
6. The process for preparing topramezone intermediate by using the supergravity reaction according to claim 1, wherein the reaction temperature in the supergravity reactor is 30-80 ℃.
7. The method for preparing topramezone intermediate by using the supergravity reaction according to claim 1, wherein the reaction pressure inside the supergravity reactor is 0.5-5 MP.
8. The method for preparing topramezone intermediate by using the supergravity reaction according to claim 1, wherein the rotating speed of the rotating body is 300-1200 r/min.
9. The process for preparing topramezone intermediate by using a hypergravity reaction as claimed in claim 1, wherein the filler layer (10) comprises one or a mixture of two or more of silica, titania, magnesia and carbon.
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