DESC:FIELD
The present disclosure relates to a process for the purification of Chlorantraniliprole.
BACKGROUND
The background information herein below relates to the present disclosure but is not necessarily prior art.
Chlorantraniliprole is a broad-spectrum anthranilic diamide insecticide. Chlorantraniliprole, when consumed by insects, it interrupts normal muscle contraction, resulting in the death of the insects. The structural formula for Chlorantraniliprole is given below.

(I)
Various methods for the preparation of Chlorantraniliprole are known in the art, however, known methods provide Chlorantraniliprole with impurities. Further, the impurities in Chlorantraniliprole may affect the efficacy, safety, and stability of the final product. It is desired to purify crude Chlorantraniliprole to obtain the specified purity required for commercial applications.
Conventional methods for the purification of Chlorantraniliprole provide Chlorantraniliprole with low yield. Further, the conventional methods required a large amount of solvent for multiple washing thereby increasing the overall cost of the purification.
Therefore, there is felt a need to provide a process for the purification of Chlorantraniliprole that mitigates the aforestated drawbacks or at least provides a suitable alternative.
OBJECTS
Some of the objects of the present disclosure, which at least one embodiment herein satisfies, are as follows:
It is an object of the present disclosure to ameliorate one or more problems of the background or to at least provide a useful alternative.
Another object of the present disclosure is to provide a process for the purification of Chlorantraniliprole.
Yet another object of the present disclosure is to provide a process for the purification of Chlorantraniliprole that is simple and cost-efficient.
Still another object of the present disclosure is to provide a process for the purification of Chlorantraniliprole that provides high yield and purity of Chlorantraniliprole.
Other objects and advantages of the present disclosure will be more apparent from the following description, which is not intended to limit the scope of the present disclosure.
SUMMARY
The present disclosure relates to a process for the purification of Chlorantraniliprole. The process comprises mixing a predetermined amount of crude Chlorantraniliprole with a predetermined amount of at least one first fluid medium under stirring and heated to a first predetermined temperature for a first predetermined time period to obtain a mixture. The mixture is cooled to a second predetermined temperature to obtain a cooled mixture. The cooled mixture is filtered to obtain a first wet cake. The so obtained first wet cake is washed at least twice with a second fluid medium to obtain a second wet cake. The second wet cake is optionally mixed with a third fluid medium under stirring at a third predetermined temperature for a second predetermined time period to obtain a slurry, followed by filtration to obtain a third wet cake. The so obtained third wet cake is optionally washed with a fourth fluid medium at least twice followed by drying at a fourth predetermined temperature to obtain pure Chlorantraniliprole.
In an embodiment, the first fluid medium is at least one selected from the group consisting of acetic acid, aqueous acetic acid, toluene, N-methyl pyrrolidinone, and water.
In an embodiment of the present disclosure, the ratio of the crude Chlorantraniliprole to the first fluid medium is in the range of 1:2 w/v to 1:5 w/v.
In an embodiment, the first predetermined temperature is in the range of 40°C to 100°C.
In an embodiment of the present disclosure, the first predetermined time period is in the range of 30 minutes to 120 minutes.
In an embodiment of the present disclosure, the second predetermined temperature is in the range of 20°C to 40°C.
In an embodiment of the present disclosure, the second fluid medium is at least one selected from the group consisting of acetic acid, aqueous acetic acid, toluene, N-methyl pyrrolidinone, and water.
In an embodiment of the present disclosure, the third fluid medium is water.
In an embodiment of the present disclosure, the third predetermined temperature is in the range of 20°C to 40°C.
In an embodiment of the present disclosure, wherein said second predetermined time period is in the range of 30 minutes to 120 minutes.
In an embodiment of the present disclosure, the fourth fluid medium is water.
In an embodiment of the present disclosure, the fourth predetermined temperature is in the range of 50°C to 70°C.
In an embodiment of the present disclosure, the purity of Chlorantraniliprole is in the range of 97% to 99%.
DETAILED DESCRIPTION
The present disclosure relates to a process for the purification of Chlorantraniliprole.
Embodiments, of the present disclosure, will now be described herein. Embodiments are provided so as to thoroughly and fully convey the scope of the present disclosure to the person skilled in the art. Numerous details are set forth, relating to specific components, and methods, to provide a complete understanding of embodiments of the present disclosure. It will be apparent to the person skilled in the art that the details provided in the embodiments should not be construed to limit the scope of the present disclosure. In some embodiments, well-known processes, well-known apparatus structures, and well-known techniques are not described in detail.
The terminology used, in the present disclosure, is only for the purpose of explaining a particular embodiment and such terminology shall not be considered to limit the scope of the present disclosure. As used in the present disclosure, the forms "a,” "an," and "the" may be intended to include the plural forms as well, unless the context clearly suggests otherwise. The terms "comprises," "comprising," “including,” and “having,” are open ended transitional phrases and therefore specify the presence of stated features, integers, steps, operations, elements, modules, units and/or components, but do not forbid the presence or addition of one or more other features, integers, steps, operations, elements, components, and/or groups thereof. The particular order of steps disclosed in the method and process of the present disclosure is not to be construed as necessarily requiring their performance as described or illustrated. It is also to be understood that additional or alternative steps may be employed.
As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed elements.
The terms first, second, third, etc., should not be construed to limit the scope of the present disclosure as the aforementioned terms may be only used to distinguish one element, component, region, layer or section from another component, region, layer or section. Terms such as first, second, third etc., when used herein do not imply a specific sequence or order unless clearly suggested by the present disclosure.
Chlorantraniliprole is a broad-spectrum anthranilic diamide insecticide. Chlorantraniliprole, when consumed by insects, it interrupts normal muscle contraction, resulting in the death of the insects. The structural formula for Chlorantraniliprole is given below.

(I)
Various methods for the preparation of Chlorantraniliprole are known in the art, however, known methods provide Chlorantraniliprole with impurities. Further, the impurities in Chlorantraniliprole may affect the efficacy, safety, and stability of the final product. It is desired to purify crude Chlorantraniliprole to obtain the specified purity required for commercial applications.
Conventional methods for the purification of Chlorantraniliprole provide Chlorantraniliprole with a low yield. Further, the conventional methods required a large amount of solvent for multiple washing thereby increasing the overall cost of the purification.
The present disclosure provides a process for the purification of Chlorantraniliprole. The process of the present disclosure is simple, environment friendly, efficiently removes the majority of the impurities, and provides higher purity and better yield of Chlorantraniliprole.
In an aspect of the present disclosure, there is provided a process for the purification of Chlorantraniliprole.
The process for the purification of Chlorantraniliprole is described in detail below.
In a first step, a predetermined amount of crude Chlorantraniliprole is mixed with a predetermined amount of at least one first fluid medium under stirring and heated to a first predetermined temperature for a first predetermined time period to obtain a mixture.
In an embodiment of the present disclosure, the first fluid medium is at least one selected from the group consisting of acetic acid, aqueous acetic acid, toluene, N-methyl pyrrolidinone, and water. In an exemplary embodiment of the present disclosure, the first fluid medium is aqueous acetic acid. In another exemplary embodiment of the present disclosure, the first fluid medium is acetic acid. In still another exemplary embodiment of the present disclosure, the first fluid medium is N-methyl pyrrolidinone. In yet another exemplary embodiment of the present disclosure, the first fluid medium is a mixture of acetic acid and toluene.
In an embodiment of the present disclosure, the ratio of the crude Chlorantraniliprole to the first fluid medium is in the range of 1:2 w/v to 1:5 w/v. In an exemplary embodiment of the present disclosure, the ratio of the crude Chlorantraniliprole to the first fluid medium is 1:3 w/v.
In an embodiment of the present disclosure, the first predetermined temperature is in the range of 40°C to 100°C. In an exemplary embodiment of the present disclosure, the first predetermined temperature is 40°C. In another exemplary embodiment of the present disclosure, the first predetermined temperature is 45°C. In yet another exemplary embodiment of the present disclosure, the first predetermined temperature is 75°C. In still another exemplary embodiment of the present disclosure, the first predetermined temperature is 80°C.
In an embodiment of the present disclosure, the first predetermined time period is in the range of 30 minutes to 120 minutes. In an exemplary embodiment of the present disclosure, the first predetermined time period is 60 minutes.
In a second step, the mixture is cooled to a second predetermined temperature to obtain a cooled mixture.
In an embodiment of the present disclosure, the second predetermined temperature is in the range of 20°C to 40°C. In an exemplary embodiment of the present disclosure, the second predetermined temperature is 27°C. In another exemplary embodiment of the present disclosure, the second predetermined temperature is 34°C.
In a third step, the cooled mixture is filtered to obtain a first wet cake.
In a fourth step, the first wet cake is washed with a second fluid medium at least twice followed by filtration to obtain a second wet cake.
In an embodiment of the present disclosure, the second fluid medium is at least one selected from the group consisting of acetic acid, aqueous acetic acid, toluene, N-methyl pyrrolidinone, and water. In an exemplary embodiment of the present disclosure, the second fluid medium is aqueous acetic acid. In another exemplary embodiment of the present disclosure, the second fluid medium is acetic acid. In still another exemplary embodiment of the present disclosure, the second fluid medium is N-methyl pyrrolidinone. In yet another exemplary embodiment of the present disclosure, the second fluid medium is a mixture of acetic acid and toluene.
In a fifth step, optionally a second wet cake is mixed with a third fluid medium under stirring at a third predetermined temperature for a second predetermined time period to obtain a slurry, followed by filtration to obtain a third wet cake.
In an embodiment of the present disclosure, the third fluid medium is water.
In an embodiment of the present disclosure, the third predetermined temperature is in the range of 20°C to 40°C. In an exemplary embodiment of the present disclosure, the third predetermined temperature is 27°C. In an exemplary embodiment of the present disclosure, the third predetermined temperature is 34°C.
In an embodiment of the present disclosure, the second predetermined time period is in the range of 30 minutes to 120 minutes. In an exemplary embodiment of the present disclosure, the second predetermined time period is 60 minutes.
In the final step, optionally a third wet cake is washed with a fourth fluid medium at least twice followed by drying at a fourth predetermined temperature to obtain pure Chlorantraniliprole.
In an embodiment of the present disclosure, the fourth fluid medium is water.
In an embodiment of the present disclosure, the fourth predetermined temperature is in the range of 50°C to 70°C. In an exemplary embodiment of the present disclosure, the fourth predetermined temperature is 58°C.
In an embodiment of the present disclosure, the recovery of Chlorantraniliprole is in the range of 77% to 96%.
The term ‘recovery’ in the present disclosure denotes the amount of the product recovered (yield) from the crude Chlorantraniliprole. The term suitably indicates the process of purification and differentiates from the synthesis.
In an embodiment of the present disclosure, the purity of Chlorantraniliprole is in the range of 97% to 99%.
The foregoing description of the embodiments has been provided for purposes of illustration and is not intended to limit the scope of the present disclosure. Individual components of a particular embodiment are generally not limited to that particular embodiment, but, are interchangeable. Such variations are not to be regarded as a departure from the present disclosure, and all such modifications are considered to be within the scope of the present disclosure.
The present disclosure is further described in light of the following experiments which are set forth for illustration purposes only and not to be construed for limiting the scope of the disclosure. The following experiments are scalable to industrial/commercial processes.
EXPERIMENTAL DETAILS
EXPERIMENT 1: Process for the preparation of Chlorantraniliprole

183 gm of 3-Bromo-1-(3-chloro-2-pyridinyl)-1H-pyrazole-5-carboxylic acid was charged into a reactor followed by adding 1200 ml of acetonitrile under stirring at 30°C for 10 minutes to obtain a first mixture. 83 gm of sodium carbonate was added to the first mixture under stirring followed by adding/rinsing 180 ml of acetonitrile to obtain a second mixture. The second mixture was equilibrated at 30°C for 30 minutes to obtain a third mixture. 82.4 gm of methanesulfonyl chloride was added to the third mixture under stirring at 30°C for 1 hour to obtain a fourth mixture. The fourth mixture was equilibrated for 45 minutes to obtain a first reaction mass.
Separately, 117.8 gm of 2-amino-5-chloro-3-methylbenzoic acid was mixed with 600 ml of acetonitrile to obtain a slurry. The so obtained slurry was mixed with a first reaction mass slowly under stirring for 1 hour to obtain a mass. The so obtained mass was equilibrated at 30°C for 1 hour followed by adding 41.5 gm of sodium carbonate (first portion) and 90 ml of acetonitrile to obtain a second reaction mass.
To the second reaction mass, 41.2 gm of methanesulfonyl chloride (first portion) was added slowly over a period of 30 minutes to 40 minutes followed by adding 20.75 gm of sodium carbonate (second portion) and 45 ml of acetonitrile to obtain a first resultant mixture. Maintaining the temperature of the first resultant mixture at 25°C to 35°C, 20.6 gm of methanesulfonyl chloride (second portion) was added slowly to the first resultant mixture for 30 minutes followed by adding 20.75 gm of sodium carbonate (third portion) and 45 ml of acetonitrile to obtain a second resultant mixture. 20.6 gm of methanesulfonyl chloride (third portion) was slowly added to the second resultant mixture for 30 minutes followed by adding 240 ml of acetonitrile to obtain a third resultant mixture. The third resultant mixture was equilibrated at 25°C to 35°C to obtain a fourth resultant mixture comprising 6-chloro-2-(3-bromo-1-(3-chloropyridin-2-yl)-1Hpyrazol-5-yl)-8-methyl-4H-benzo[d][1,3] oxazin-4-one and 3-bromo-1-(3-chloro-2-pyridinyl)-1H-pyrazole-5-carboxylic acid.
The reaction was monitored by HPLC. When the amount of 3-bromo-1-(3-chloro-2-pyridinyl)-1H-pyrazole-5-carboxylic acid in the fourth resultant mixture was observed <2%, methylamine gas was bubbled below the surface of the fourth resultant mixture at 25°C to 30°C to obtain a resultant mass.
The resultant mass was filtered and washed twice with 100 ml of acetonitrile to obtain a wet cake (794 gm). The wet cake was suck dried and slurried in 600 ml of water under stirring at 25°C to 35°C for 1 hour to obtain a product slurry. The product slurry was washed twice with 100 ml of water and suck dried to obtain the crude Chlorantraniliprole.
The yield of the crude Chlorantraniliprole was 91.82% (319 gm), HPLC purity was 97.5%, LOD (limit of detection) was 13.34% wt/wt.
EXPERIMENT 2: Purification of Chlorantraniliprole
319 gm of crude Chlorantraniliprole was charged into a reactor followed by adding 925 ml of aqueous acetic acid (94% acetic acid concentration) and heated to 50°C under stirring for 1 hour to obtain a mixture. The mixture was cooled to 27°C under stirring to obtain a cooled mixture. The cooled mixture was filtered to obtain a wet cake and a filtrate. The so obtained first wet cake was washed twice with 100 ml (each) of aqueous acetic acid (90% acetic acid concentration) to obtain a second wet cake. The second wet cake was slurried in 600 ml of water under stirring at 27°C for 1 hour to obtain a slurry. The slurry was filtered to obtain a third wet cake. The third wet cake was washed twice with 150 ml (each) of water followed by drying at 55°C to obtain Chlorantraniliprole.
The yield/recovery of the Chlorantraniliprole was 77.11% (246 gm), and the HPLC purity was 97.96%.
EXPERIMENT 3: Purification of Chlorantraniliprole
50 gm of crude Chlorantraniliprole (HPLC purity = 96.6%) was charged into a reactor followed by adding 150 ml of aqueous acetic acid (95% acetic acid concentration) and heated to 75°C under stirring for 1 hour to obtain a mixture. The mixture was cooled to 27°C under stirring to obtain a cooled mixture. The cooled mixture was filtered to obtain a first wet cake and a filtrate. The so obtained first wet cake was washed twice with 25 ml (each) of aqueous acetic acid (95% acetic acid concentration) to obtain a second wet cake. The second wet cake was slurried in 150 ml of water under stirring at 27°C for 1 hour to obtain a slurry. The slurry was filtered to obtain a third wet cake. The third wet cake was washed twice with 50 ml of water followed by drying at 58°C to obtain Chlorantraniliprole.
The yield/recovery of Chlorantraniliprole was 82% (41 gm), and the HPLC purity was 99%.
EXPERIMENT 4: Purification of Chlorantraniliprole
360 gm of crude Chlorantraniliprole (HPLC purity = 96.23%) was charged into a reactor followed by adding 1080 ml of acetic acid and heated to 45°C under stirring for 1 hour to obtain a mixture. The mixture was cooled to 27°C under stirring to obtain a cooled mixture. The cooled mixture was filtered to obtain a first wet cake and a filtrate. The so obtained first wet cake was washed twice with 100 ml (each) of acetic acid to obtain a second wet cake. The second wet cake was slurried in 400 ml of water under stirring at 27°C for 1 hour to obtain a slurry. The slurry was filtered to obtain a third wet cake. The third wet cake was washed twice with 200 ml (each) of water followed by drying at 57°C to obtain Chlorantraniliprole.
The yield/recovery of the Chlorantraniliprole was 89.72% (323 gm), and the HPLC purity was 97.66%.
EXPERIMENT 5: Purification of Chlorantraniliprole
50 gm of crude Chlorantraniliprole (HPLC purity = 96.6%) was charged into a reactor followed by adding 150 ml of acetic acid-toluene mixture (80:20 acetic acid: toluene v/v) and heated to 75°C under stirring for 1 hour to obtain a mixture. The mixture was cooled to 27°C under stirring to obtain a cooled mixture. The cooled mixture was filtered to obtain a first wet cake and a filtrate. The so obtained first wet cake was washed twice with 25 ml (each) of acetic acid-toluene mixture (80:20 v/v) to obtain a second wet cake. The second wet cake was slurried in 150 ml of water under stirring and heated at 27°C for 1 hour to obtain a slurry. The slurry was filtered to obtain a third wet cake. The third wet cake was washed twice with 25 ml (each) of water followed by drying at 60°C to obtain Chlorantraniliprole.
The yield/recovery of the Chlorantraniliprole was 86% (43 gm), and the HPLC purity was 98.61%.
EXPERIMENT 6: Purification of Chlorantraniliprole
50 gm of crude Chlorantraniliprole (HPLC purity = 96.6%) was charged into a reactor followed by adding 150 ml of N-methyl pyrrolidinone and heated to 40°C under stirring for 1 hour to obtain a mixture (clear solution). The first mixture (clear solution) was cooled to 27°C followed by adding 65 ml of water under stirring to obtain a precipitated mixture. The precipitated mixture was filtered to obtain a wet cake and a filtrate. The wet cake was washed twice with 50 ml (each) of water followed by drying at 56°C to obtain Chlorantraniliprole.
The yield/recovery of the Chlorantraniliprole was 92% (46 gm), and the HPLC purity was 98.21%.
EXPERIMENT 7: Purification of Chlorantraniliprole
50 gm of crude Chlorantraniliprole (HPLC purity = 96.6%) was charged into a reactor followed by adding 150 ml of acetic acid-toluene mixture (80:20 v/v) and heated to 75°C under stirring for 1 hour to obtain a mixture. The mixture was cooled to 27°C under stirring to obtain a cooled mixture. The cooled mixture was filtered to obtain a wet cake and a filtrate. The wet cake was washed twice with 30 ml of acetic acid-toluene mixture (80:20 v/v) followed by drying at 56°C to obtain Chlorantraniliprole.
The yield/recovery of Chlorantraniliprole was 94% (47 gm), and the HPLC purity was 97.91%.
EXPERIMENT 8: Purification of Chlorantraniliprole
100 gm of crude Chlorantraniliprole (HPLC purity = 96.23%) was charged into a reactor followed by adding 300 ml of acetic acid and heated to 50°C under stirring for 1 hour to obtain a mixture. The mixture was cooled to 34°C under stirring to obtain a cooled mixture. The cooled mixture was filtered to obtain a first wet cake and a filtrate. The so obtained first wet cake was washed twice with 50 ml (each) of acetic acid to obtain a second wet cake. The second wet cake was slurried in 400 ml of water under stirring at 34°C for 1 hour to obtain a slurry. The slurry was filtered to obtain a third wet cake. The third wet cake was washed twice with 100 ml (each) of water followed by drying at 58°C to obtain Chlorantraniliprole.
The yield/recovery of the Chlorantraniliprole was 90% (90 gm), and the HPLC purity was 98%.
EXPERIMENT 9: Purification of Chlorantraniliprole
75 gm of crude Chlorantraniliprole (HPLC purity = 96.6%) was charged into a reactor followed by adding 225 ml of acetic acid-toluene mixture (80:20 acetic acid: toluene v/v) and heated to 80°C under stirring for 1 hour to obtain a mixture. The mixture was cooled to 34°C under stirring to obtain a cooled mixture. The cooled mixture was filtered to obtain a first wet cake and a filtrate. The so obtained first wet cake was washed twice with 40 ml (each) of acetic acid-toluene mixture (80:20 v/v) to obtain a second wet cake. The second wet cake was slurried in 225 ml of water under stirring and heated at 34°C for 1 hour to obtain a slurry. The slurry was filtered to obtain a third wet cake. The third wet cake was washed twice with 40 ml (each) of water followed by drying at 60°C to obtain Chlorantraniliprole.
The yield/recovery of the Chlorantraniliprole was 86.5% (64.88 gm), and the HPLC purity was 98.5%.
EXPERIMENT 10: Purification of Chlorantraniliprole
100 gm of crude Chlorantraniliprole (HPLC purity = 96.6%) was charged into a reactor followed by adding 300 ml of N-methyl pyrrolidinone and heated to 45°C under stirring for 1 hour to obtain a mixture (clear solution). The first mixture (clear solution) was cooled to 34°C followed by adding 100 ml of water under stirring to obtain a precipitated mixture. The precipitated mixture was filtered to obtain a wet cake and a filtrate. The wet cake was washed twice with 100 ml (each) of water followed by drying at 57°C to obtain Chlorantraniliprole.
The yield/recovery of the Chlorantraniliprole was 91.8% (91.8 gm), and the HPLC purity was 98%.
EXPERIMENT 11: Purification of Chlorantraniliprole
150 gm of crude Chlorantraniliprole (HPLC purity = 96.6%) was charged into a reactor followed by adding 450 ml of acetic acid-toluene mixture (80:20 v/v) and heated to 80°C under stirring for 1 hour to obtain a mixture. The mixture was cooled to 34°C under stirring to obtain a cooled mixture. The cooled mixture was filtered to obtain a wet cake and a filtrate. The wet cake was washed twice with 100 ml of acetic acid-toluene mixture (80:20 v/v) followed by drying at 55°C to obtain Chlorantraniliprole.
The yield/recovery of the Chlorantraniliprole was 94.7% (142 gm), and the HPLC purity was 98%.
TECHNICAL ADVANCEMENT
The present disclosure described hereinabove has several technical advantages including, but not limited to, the realization of a process for the purification of Chlorantraniliprole, that:
• is a simple and cost-effective process;
• is environment friendly; and
• provides a higher yield and higher purity of Chlorantraniliprole in comparison to conventional processes.
The embodiments herein and the various features and advantageous details thereof are explained with reference to the non-limiting embodiments in the following description. Descriptions of well-known components and processing techniques are omitted so as to not unnecessarily obscure the embodiments herein. The examples used herein are intended merely to facilitate an understanding of ways in which the embodiments herein may be practiced and to further enable those of skill in the art to practice the embodiments herein. Accordingly, the examples should not be construed as limiting the scope of the embodiments herein.
The foregoing description of the specific embodiments so fully reveal the general nature of the embodiments herein that others can, by applying current knowledge, readily modify and/or adapt for various applications such specific embodiments without departing from the generic concept, and, therefore, such adaptations and modifications should and are intended to be comprehended within the meaning and range of equivalents of the disclosed embodiments. It is to be understood that the phraseology or terminology employed herein is for the purpose of description and not of limitation. Therefore, while the embodiments herein have been described in terms of preferred embodiments, those skilled in the art will recognize that the embodiments herein can be practiced with modification within the spirit and scope of the embodiments as described herein.
The use of the expression “at least” or “at least one” suggests the use of one or more elements or ingredients or quantities, as the use may be in the embodiment of the invention to achieve one or more of the desired objects or results. While certain embodiments of the inventions have been described, these embodiments have been presented by way of example only, and are not intended to limit the scope of the inventions. Variations or modifications to the formulation of this invention, within the scope of the invention, may occur to those skilled in the art upon reviewing the disclosure herein. Such variations or modifications are well within the spirit of this invention.
Any discussion of documents, acts, materials, devices, articles or the like that has been included in this specification is solely for the purpose of providing a context for the disclosure. It is not to be taken as an admission that any or all of these matters form a part of the prior art base or were common general knowledge in the field relevant to the disclosure as it existed anywhere before the priority date of this application.
The numerical values given for various physical parameters, dimensions, and quantities are only approximate values and it is envisaged that the values higher than the numerical value assigned to the physical parameters, dimensions and quantities fall within the scope of the invention unless there is a statement in the specification to the contrary.
While considerable emphasis has been placed herein on the specific features of the preferred embodiment, it will be appreciated that many additional features can be added and that many changes can be made in the preferred embodiment without departing from the principles of the disclosure. These and other changes in the preferred embodiment of the disclosure will be apparent to those skilled in the art from the disclosure herein, whereby it is to be distinctly understood that the foregoing descriptive matter is to be interpreted merely as illustrative of the disclosure and not as a limitation.
,CLAIMS:WE CLAIM:
1. A process for the purification of Chlorantraniliprole, said process comprising the following steps:
a) mixing a predetermined amount of crude Chlorantraniliprole with a predetermined amount of at least one first fluid medium under stirring and heated to a first predetermined temperature for a first predetermined time period to obtain a mixture;
b) cooling said mixture to a second predetermined temperature to obtain a cooled mixture;
c) filtering said cooled mixture to obtain a first wet cake;
d) washing said first wet cake with a second fluid medium at least twice to obtain a second wet cake;
e) optionally mixing said second wet cake with a third fluid medium under stirring at a third predetermined temperature for a second predetermined time period to obtain a slurry, followed by filtration to obtain a third wet cake; and
f) optionally washing said third wet cake with a fourth fluid medium at least twice followed by drying at a fourth predetermined temperature to obtain pure Chlorantraniliprole.
2. The process as claimed in claim 1, wherein said first fluid medium is at least one selected from the group consisting of acetic acid, aqueous acetic acid, toluene, N-methyl pyrrolidinone, and water.
3. The process as claimed in claim 1, wherein the ratio of the crude Chlorantraniliprole to said first fluid medium is in the range of 1:2 w/v to 1:5 w/v.
4. The process as claimed in claim 1, wherein said first predetermined temperature is in the range of 40°C to 100°C.
5. The process as claimed in claim 1, wherein said first predetermined time period is in the range of 30 minutes to 120 minutes.
6. The process as claimed in claim 1, wherein said second predetermined temperature is in the range of 20°C to 40°C.
7. The process as claimed in claim 1, wherein said second fluid medium is at least one selected from the group consisting of acetic acid, aqueous acetic acid, toluene, N-methyl pyrrolidinone, and water.
8. The process as claimed in claim 1, wherein said third fluid medium is water.
9. The process as claimed in claim 1, wherein said third predetermined temperature is in the range of 20°C to 40°C.
10. The process as claimed in claim 1, wherein said second predetermined time period is in the range of 30 minutes to 120 minutes.
11. The process as claimed in claim 1, wherein said fourth fluid medium is water.
12. The process as claimed in claim 1, wherein said fourth predetermined temperature is in the range of 50°C to 70°C.
13. The process as claimed in claim 1, wherein the purity of Chlorantraniliprole is in the range of 97% to 99%.

Dated this 15th Day of November, 2023

_______________________________
MOHAN RAJKUMAR DEWAN, IN/PA – 25
of R.K. DEWAN & CO.
Authorized Agent of Applicant