CN117229221A - Purification method of bupirimate - Google Patents
Purification method of bupirimate Download PDFInfo
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- CN117229221A CN117229221A CN202311023073.8A CN202311023073A CN117229221A CN 117229221 A CN117229221 A CN 117229221A CN 202311023073 A CN202311023073 A CN 202311023073A CN 117229221 A CN117229221 A CN 117229221A
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- bupirimate
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- DSKJPMWIHSOYEA-UHFFFAOYSA-N bupirimate Chemical compound CCCCC1=C(C)N=C(NCC)N=C1OS(=O)(=O)N(C)C DSKJPMWIHSOYEA-UHFFFAOYSA-N 0.000 title claims abstract description 110
- 239000005742 Bupirimate Substances 0.000 title claims abstract description 102
- 238000000034 method Methods 0.000 title claims abstract description 40
- 238000000746 purification Methods 0.000 title claims abstract description 20
- 238000001914 filtration Methods 0.000 claims abstract description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000001035 drying Methods 0.000 claims abstract description 17
- 238000001816 cooling Methods 0.000 claims abstract description 14
- 150000007522 mineralic acids Chemical class 0.000 claims abstract description 13
- 238000005904 alkaline hydrolysis reaction Methods 0.000 claims abstract description 11
- 238000005755 formation reaction Methods 0.000 claims abstract description 10
- 150000003839 salts Chemical class 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 36
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 24
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 24
- 238000006243 chemical reaction Methods 0.000 claims description 23
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 21
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 16
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 12
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 12
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 4
- 239000003960 organic solvent Substances 0.000 abstract description 11
- 238000001953 recrystallisation Methods 0.000 abstract description 9
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 238000009776 industrial production Methods 0.000 abstract description 3
- 239000002904 solvent Substances 0.000 abstract description 3
- 150000004945 aromatic hydrocarbons Chemical class 0.000 abstract 1
- 230000002349 favourable effect Effects 0.000 abstract 1
- 239000002912 waste gas Substances 0.000 abstract 1
- 239000000047 product Substances 0.000 description 15
- 238000003756 stirring Methods 0.000 description 9
- 239000012535 impurity Substances 0.000 description 8
- 238000002360 preparation method Methods 0.000 description 8
- 239000003513 alkali Substances 0.000 description 7
- 230000015572 biosynthetic process Effects 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- 238000004090 dissolution Methods 0.000 description 5
- 150000007529 inorganic bases Chemical class 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 229910021645 metal ion Inorganic materials 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 3
- 230000000844 anti-bacterial effect Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- -1 5-butyl-2-ethylamino-6-methylpyrimidinyl-4-yl dimethyl sulfamate Chemical compound 0.000 description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 239000003899 bactericide agent Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 241000221785 Erysiphales Species 0.000 description 1
- CZPWVGJYEJSRLH-UHFFFAOYSA-N Pyrimidine Chemical compound C1=CN=CN=C1 CZPWVGJYEJSRLH-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000001479 atomic absorption spectroscopy Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000002612 dispersion medium Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000008029 eradication Effects 0.000 description 1
- 239000012065 filter cake Substances 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000004811 liquid chromatography Methods 0.000 description 1
- 230000005923 long-lasting effect Effects 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 150000001455 metallic ions Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000010815 organic waste Substances 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 230000009885 systemic effect Effects 0.000 description 1
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Landscapes
- Heterocyclic Carbon Compounds Containing A Hetero Ring Having Oxygen Or Sulfur (AREA)
Abstract
The application discloses a purification method of bupirimate, which comprises the following steps: step 1: mixing the crude bupirimate with water, adding inorganic acid under cooling condition to perform salt formation reaction, and filtering to obtain crude bupirimate salt; step 2: and sequentially performing alkaline hydrolysis, filtering and drying on the crude bupirimate to obtain a refined bupirimate. Compared with the process of using organic solvent for recrystallization in the traditional process, the cost is greatly reduced; meanwhile, the problems of high solvent volatilization, high production cost, amplified emission of aromatic hydrocarbon waste gas, great harm to the environment and the like caused by the repeated multi-stage recrystallization operation of the organic solvent are avoided. Meanwhile, the technical scheme of the application is easy to operate, has relatively low purification cost, and is favorable for industrial production.
Description
Technical Field
The application belongs to the technical field of pesticide raw material preparation processes, and particularly relates to a purification method of bupirimate.
Background
Bupirimate is a novel pyrimidine agricultural bactericide, has good systemic activity, excellent protection, treatment and eradication activities and long lasting period. A large number of field efficacy tests show that the bupirimate can be quickly absorbed by plant stems and leaves and run to various parts in the plant body, and can strongly inhibit the formation and metabolism of germ spores to cause death of the germ spores, so that the treatment effect is achieved and the bupirimate has special effects on powdery mildew;
bupirimate chemical name: 5-butyl-2-ethylamino-6-methylpyrimidinyl-4-yl dimethyl sulfamate, english name: bupirimate, cas#:41483-42-6, the chemical structural formula is as follows:
with reference to DE 2246645/DE2265028/DE2265312 and Li Jingxia, the bupirimate synthesis process is optimised, journal of the university of the three-channel occupational technology, 2013, 12 (3): 115-116): the product was obtained as a pale yellow waxy solid in appearance.
CN202010816895.1 and CN202010266757.0 bupirimate, the appearance of the bupirimate obtained is light brown waxy solid.
The bupirimate prepared by the existing synthesis process contains various organic impurities and metal ion impurities introduced by raw materials and catalysts. Wherein, the existence of partial organic impurities seriously affects the efficacy and dosage of bupirimate, while the metallic ion impurities affect the storage stability of bupirimate, and affect the storage stability and efficacy when bupirimate is mixed with other bactericides, thus the bupirimate is necessary to be purified, the efficacy is improved, and the dosage risk is reduced.
In the prior art, the purification mode of the bupirimate is as follows: and dissolving the crude bupirimate with an organic solvent at a higher temperature to obtain transparent bupirimate, filtering mechanical impurities, and then cooling, crystallizing and filtering to obtain the refined bupirimate.
The method has the problems that: a. the bupirimate has the advantages of large loss, low yield and high purification cost; b. colored impurities are difficult to remove effectively, and the appearance is deep; c. the recrystallization operation is intense in stirring, long in crystallization time and not easy to operate; c. the multi-stage recrystallization operation leads to a great deal of solvent volatilization, high production cost and great harm to the environment.
Therefore, it is necessary to develop a novel purification method of bupirimate, which is easy to operate, improves yield, reduces cost, reduces influence on environment, and the like.
Disclosure of Invention
Aiming at the problems of complex process, low purity, low yield, large environmental pollution and the like of the bupirimate purification method in the prior art, the application provides the bupirimate purification method.
In order to solve the problems, the technical scheme adopted by the application comprises the following steps:
a method for purifying bupirimate, comprising: step 1: mixing the crude bupirimate with water, adding inorganic acid under cooling condition to perform salt formation reaction, and filtering to obtain crude bupirimate salt; step 2: and sequentially performing alkaline hydrolysis, filtering and drying on the crude bupirimate to obtain a refined bupirimate.
Optionally, the mass ratio of bupirimate to water in the step 1 is as follows: 1 (3-5).
Optionally, the ph=4 to 5 is finally maintained after the reaction in the step 1, and the cooling temperature is lower than 20 ℃.
Optionally, the reaction time in the step 1 is 30-45 min.
Optionally, the molar ratio of bupirimate to acid in the step 1 is 1 (0.5-1.2).
Optionally, the acid in the step 1 is at least one selected from hydrochloric acid, sulfuric acid and phosphoric acid.
Optionally, in the step 2, the molar ratio of bupirimate to alkali is as follows: 1 (0.5-1.2).
Optionally, in the step 2, the alkaline hydrolysis reaction time is 30-60 min, and finally the pH value=8-10 is maintained.
Optionally, the alkali in the step 2 is at least one selected from sodium hydroxide, potassium carbonate and potassium hydroxide.
Optionally, the temperature of the salt formation reaction of the crude bupirimate in the step 1 is 0-30 ℃; and (2) the alkaline hydrolysis temperature of the crude bupirimate in the step (2) is 0-45 ℃.
Compared with the prior art, the application has the beneficial technical effects that:
1. the process adopted by the application has large treatment capacity and high production efficiency of the bupirimate top-quality product;
2. compared with the process of using the organic solvent in the traditional process, the application improves the yield, greatly reduces the cost, greatly reduces the emission of the organic solvent and can generate larger economic benefit;
3. the inorganic acid used in the preparation of the application is sulfuric acid, phosphoric acid, phosphorous acid and hydrochloric acid; the alkali is sodium hydroxide, potassium hydroxide or potassium carbonate. All are basic chemical raw materials, are easy to obtain and have relatively low price;
4. according to the application, water is used as a dispersion medium, so that volatilization of an organic solvent is avoided, the operation environment is improved, and industrial production is facilitated;
5. compared with the traditional process using organic solvent for multiple recrystallization, the application has obviously improved product appearance and yield; meanwhile, the problems of severe stirring, long crystallization time and multistage recrystallization operation in the traditional recrystallization operation, high solvent volatilization, high production cost, amplified organic waste gas emission, great harm to the environment and the like are avoided.
6. Meanwhile, the technical scheme of the application is easy to operate and is beneficial to industrial production.
Detailed Description
In summary, the following embodiments of the present application are provided, and it should be noted that the present application is not limited to the following embodiments, and equivalent changes made on the basis of the technical solution of the present application fall within the protection scope of the present application.
The method for purifying the bupirimate without using an organic solvent is provided, and the characteristics of easy formation of salts with acid of bupirimate are utilized, the salts have low solubility in water, the bupirimate salts and impurities are well separated by filtration, and then alkaline hydrolysis is carried out at low temperature, so that the bupirimate is dissociated out, and the high-purity crude drug is obtained.
Fully mixing the crude bupirimate with metering water, adding inorganic acid under cooling condition to carry out salt formation reaction, filtering to obtain bupirimate salt, and discharging impurities and filtrate; then the bupirimate is subjected to alkaline hydrolysis, filtration and drying, so that the bupirimate refined product is obtained.
The application develops a novel purification method of bupirimate, which is simple to operate, improves the yield and purity, reduces the cost and reduces the negative influence on the environment.
The bupirimate purifying process includes the following steps:
(1) Adding crude bupirimate and water into a reaction kettle for mixing, opening jacket circulating water for cooling, dripping inorganic acid for salifying reaction, and filtering to obtain bupirimate salt
(2) And (3) carrying out alkaline hydrolysis, filtering and drying on the bupirimate salt to obtain bupirimate refined products.
Wherein, the preparation process is as follows:
a. adding crude bupirimate into the mixture according to the mass ratio of 1: 3-5, stirring, starting jacket circulating water, maintaining the temperature at not higher than 20 ℃, dropwise adding inorganic acid with the molar equivalent ratio of 1:0.5-1.2, finally keeping the pH value at 4-5, keeping stirring for 30-45 minutes, fully salifying, and filtering to obtain bupirimate salt;
b. adding alkali into bupirimate salt in the above steps, finally maintaining the pH value to be 8-10, reacting for 30-60 minutes, and filtering.
c. Washing the filter cake with water with the mass multiple of 1-2, filtering and drying to obtain the bupirimate refined product.
Further, the salt formation temperature of the crude bupirimate in the step (2) is 0-20 ℃, and the salt formation time is 30-45 minutes.
Further, the alkaline hydrolysis temperature of the crude bupirimate in the step (2) is 0-45 ℃.
Further, the inorganic acid is one or more of sulfuric acid, hydrochloric acid and phosphoric acid.
Further, the alkali is one or more of sodium hydroxide, potassium hydroxide and potassium carbonate.
The bupirimate prepared by the process has the purity of more than or equal to 98.5 percent and the yield of more than or equal to 96 percent.
Example 1:
the bupirimate purifying process includes the following steps:
(1) Sulfuric acid is used as the inorganic acid, and sodium hydroxide is used as the inorganic base;
(2) And (3) salifying the crude bupirimate with sulfuric acid, adding sodium hydroxide after complete dissolution, separating out a product, filtering and drying to obtain a refined bupirimate.
The preparation process comprises the following steps:
a. sequentially adding crude bupirimate and water (mass ratio of 1:4) into a reaction kettle, starting stirring, opening circulating water for cooling, dropwise adding sulfuric acid with a molar ratio of 1:0.55, controlling the reaction end point pH of 4-5 at the system temperature of lower than 20 ℃, reacting for 45 minutes, and filtering;
b. adding sodium hydroxide equivalent to sulfuric acid, controlling the pH at the end point of the reaction to 8-9, and controlling the temperature to be lower than 45 ℃. Reacting for 40 minutes;
e. filtering and drying;
example 2:
the bupirimate purifying process includes the following steps:
(1) The inorganic acid uses hydrochloric acid, and the inorganic base uses sodium hydroxide;
(2) And (3) salifying the crude bupirimate with hydrochloric acid, adding alkali after complete dissolution, separating out a product, filtering and drying to obtain the purified bupirimate.
The preparation process comprises the following steps:
a. adding crude bupirimate and water (mass ratio of 1:3) into a reaction kettle, starting stirring, opening circulating water for cooling, dropwise adding hydrochloric acid with a molar ratio of 1:1.08 at a system temperature lower than 20 ℃, controlling the pH of a reaction end point to be 4-5, reacting for 35 minutes, and filtering;
b. adding sodium hydroxide equivalent to hydrochloric acid, controlling the pH of the reaction end point to be 9-10, controlling the temperature to be lower than 45 ℃ and reacting for 30-45 minutes;
e. after the reaction is completed, filtering and drying;
example 3:
the bupirimate purifying process includes the following steps:
(1) The inorganic acid uses hydrochloric acid, and the inorganic base uses potassium carbonate;
(2) And (3) salifying the crude bupirimate with hydrochloric acid, adding potassium carbonate after complete dissolution, separating out a product, filtering, and drying to obtain the purified bupirimate.
The preparation process comprises the following steps:
a. adding crude bupirimate and water (mass ratio of 1:3) into a reaction kettle, starting stirring, opening circulating water for cooling, dropwise adding hydrochloric acid with a molar ratio of 1:1.08 at a system temperature lower than 20 ℃, controlling the pH of a reaction end point to be 4-5, reacting for 35 minutes, and filtering;
b. adding sodium hydroxide equivalent to hydrochloric acid, controlling the pH at the end point of the reaction to 9-10, and reacting for 30 minutes at the temperature lower than 45 ℃;
e. after the reaction is completed, filtering and drying;
example 4:
the bupirimate purifying process includes the following steps:
(1) Phosphoric acid is used as the inorganic acid, and potassium hydroxide is used as the inorganic base;
(2) And (3) salifying the crude bupirimate with phosphoric acid (the mass ratio is 1:5), adding potassium hydroxide after complete dissolution, separating out a product, filtering and drying to obtain a refined bupirimate.
The preparation process comprises the following steps:
a. adding crude bupirimate and water into a reaction kettle, starting stirring, opening circulating water for cooling, dropwise adding phosphoric acid with the molar ratio of 1:1.04, controlling the system temperature to be lower than 20 ℃, controlling the pH of a reaction end point to be 4-5, reacting for 45 minutes, and filtering;
b. adding potassium hydroxide equivalent to phosphoric acid, controlling the pH at the end point of the reaction to 9-10, and reacting for 40 minutes at the temperature lower than 45 ℃;
e. after the reaction is completed, filtering and drying;
example 5:
the bupirimate purifying process includes the following steps:
(1) The inorganic acid uses phosphoric acid, and the inorganic base uses sodium hydroxide;
(2) And (3) salifying the crude bupirimate with phosphoric acid, adding alkali after complete dissolution, separating out a product, filtering and drying to obtain the purified bupirimate.
The preparation process comprises the following steps:
a. adding crude bupirimate and water (mass ratio of 1:5) into a reaction kettle, starting stirring, opening circulating water for cooling, and enabling the system temperature to be lower than 20 ℃. Dropwise adding phosphoric acid with the molar ratio of 1:0.56, controlling the pH of the reaction end point to be 4-5, reacting for 45 minutes, and filtering;
b. adding sodium hydroxide equivalent to phosphoric acid, controlling the pH at the end point of the reaction to 9-10, and reacting for 30 minutes at the temperature lower than 45 ℃;
e. after the reaction is completed, filtering and drying;
the comparative example uses the technique described in the background: dissolving the crude bupirimate with n-heptane (mass ratio of 1:5), cooling, crystallizing at low temperature, filtering, performing tertiary recrystallization, and drying to obtain bupirimate fine product.
Detection analysis
All examples and comparative examples of the present application used the same batch of crude bupirimate as the starting material, with a purity of 92.1% and a light brown wax appearance.
1. Purity: the bupirimate prepared in each example and comparative example was tested for purity by liquid chromatography;
2. yield: the yield is the finished bupirimate product/crude bupirimate product finally prepared;
yield (%) = [ quality of refined bupirimate purity ]/[ quality of crude bupirimate purity ] x100%
3. Metal ion content: the metal ion content of bupirimate prepared in each example and comparative example was measured by atomic absorption spectrometry. The lower the content of metal ions is, the insoluble substances of acetone can be effectively reduced, the bactericidal activity of the product is improved, and the storage stability and the mixed efficacy stability are improved.
TABLE 1 purification process test results
| Sample of | Purity (%) | Yield (%) | Appearance of |
| Example 1 | 97.2 | 95.4 | White powder |
| Example 2 | 98.5 | 94.8 | White powder |
| Example 3 | 98.7 | 95.5 | White powder |
| Example 4 | 98.0 | 96.2 | White powder |
| Example 5 | 98.3 | 95.6 | White powder |
| Comparison (organic solvent) | 98.2 | 86.5 | White-like powder |
From the table above, the application improves the appearance, purity and yield of bupirimate obviously. Meanwhile, the application adopts the process to produce the high efficiency; the production cost is reduced. Compared with the traditional process that an organic solvent is used for multiple recrystallization, the purification yield and appearance of bupirimate are effectively improved; the process is easy to operate, the production efficiency is high, and the production cost is reduced; the emission of organic solvents is reduced, the harm to the environment is small, and the workshop operation environment is improved;
the preferred embodiments of the present disclosure have been described in detail above, but the present disclosure is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solutions of the present disclosure within the scope of the technical concept of the present disclosure, and all the simple modifications belong to the protection scope of the present disclosure.
In addition, the specific features described in the foregoing embodiments may be combined in any suitable manner, and in order to avoid unnecessary repetition, the present disclosure does not further describe various possible combinations.
Moreover, any combination between the various embodiments of the present disclosure is possible as long as it does not depart from the spirit of the present disclosure, which should also be construed as the disclosure of the present disclosure.
Claims (10)
1. A method for purifying bupirimate, comprising:
step 1: mixing the crude bupirimate with water, adding inorganic acid under cooling condition to perform salt formation reaction, and filtering to obtain crude bupirimate salt;
step 2: and sequentially performing alkaline hydrolysis, filtering and drying on the crude bupirimate to obtain a refined bupirimate.
2. The purification method of bupirimate according to claim 1, wherein the mass ratio of bupirimate to water in step 1 is: 1 (3-5).
3. The purification process of bupirimate according to claim 1 or 2, characterized in that the final ph=4-5 is maintained after the reaction in step 1, and the cooling temperature is lower than 20 ℃.
4. The purification method of bupirimate according to claim 1 or 2, characterized in that the reaction time in step 1 is 30-45 min.
5. The purification method of bupirimate according to claim 1 or 2, characterized in that the molar ratio of bupirimate to acid in step 1 is 1 (0.5-1.2).
6. The method for purifying bupirimate according to claim 1 or 2, wherein the acid in step 1 is at least one selected from the group consisting of hydrochloric acid, sulfuric acid and phosphoric acid.
7. The purification method of bupirimate according to claim 1 or 2, wherein the molar ratio of bupirimate to base in step 2 is: 1 (0.5-1.2).
8. The purification method of bupirimate according to claim 1 or 2, characterized in that the alkaline hydrolysis reaction time in step 2 is 30-60 min, and finally the pH value=8-10 is maintained.
9. The method for purifying bupirimate according to claim 1 or 2, characterized in that the base in step 2 is at least one selected from the group consisting of sodium hydroxide, potassium carbonate and potassium hydroxide.
10. The purification method of bupirimate according to claim 1 or 2, characterized in that the temperature of the crude bupirimate salt formation reaction in step 1 is 0-30 ℃;
and (2) the alkaline hydrolysis temperature of the crude bupirimate in the step (2) is 0-45 ℃.
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