Method of purifying a pesticide 机翻标题: 暂无翻译,请尝试点击翻译按钮。

公开号/公开日
US2003199394 A1 2003-10-23 [US20030199394]US7247175 B2 2007-07-24 [US7247175] / 2003-10-232007-07-24
申请号/申请日
2003US-10397765 / 2003-03-26
发明人
FINCH CHARLES W;FERSCH KENNETH E;
申请人
BASF;
主分类号
IPC分类号
A01N-025/14A01N-025/26A01N-047/20A01N-047/24B01D-009/00C07D-231/22
摘要
(US7247175) The present invention describes a method of purifying a pesticide that includes: a) melting a pesticide, wherein the pesticide includes at least one active ingredient and at least one impurity capable of inhibiting crystallization; b) coating the pesticide on a substrate to form a pesticide particle; c) substantially reducing the amount of crystallization inhibiting impurity by an azeotropic method; and d) crystallizing the pesticide.  In another embodiment, the present invention includes a method of purifying a pesticide as described above, such that the pesticide has a melting point of not more than about 90° C.  Also included in the invention is the product produced by the above process for the pesticide, methyl N-(2-{[1-(4-chlorophenyl)-1H-pyrazol-3-yl]oxymethyl}phenyl)N-methoxy carbamate.
机翻摘要
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地址
代理人
代理机构
;
优先权号
2002US-60368411 2002-03-28 2003US-10397765 2003-03-26
主权利要求
(US7247175) What is claimed is: 1.  A method of purifying a pesticide comprising:     a) melting a pesticide, wherein the pesticide comprises at least one active ingredient and at least one impurity capable of inhibiting crystallization;  b) coating the melted pesticide on a substrate to form a pesticide particle;c) substantially reducing the amount of crystallization inhibiting impurity by an azeotropic method;  and    d) crystallizing the pesticide. 2. The method of claim 1, wherein the active ingredient is a compound of formula (I): wherein - - - - is a single or double bond and the indices and the substituents have the following meanings: n is 0, 1, 2, 3 or 4, it being possible for the substituents R1 to be different if n is greater than 1;  m is 0, 1 or 2, it being possible for the substituents R2 to be different if m is greater than 1;X is a direct bond, 0 or NRa;Ra is hydrogen, alkyl, alkenyl, alkynyl, cycloalkyl or cycloalkenyl;R1 is nitro, cyano, halogen, unsubstituted or substituted alkyl, alkenyl, alkynyl, alkoxy, alkenyloxy, alkynyloxy or in the case where n is 2, additionally is an unsubstituted or substituted bridge bonded to two adjacent ring atoms and containing three to four members from the group consisting of 3 or four carbon atoms, 1 to 3 carbon atoms and 1 or 2 nitrogen, oxygen and/or sulfur atoms, this bridge together with the ring to which it is bonded being able to form a partly unsaturated or aromatic radical;R2 is nitro, cyano, halogen, alkyl, haloalkyl, alkoxy, alkylthio or alkoxycarbonyl;R3 unsubstituted or substituted alkyl, alkenyl or alkynyl;  an unsubstituted or substituted, saturated or mono or diunsaturated ring which, in addition to carbon atoms, can contain one to three of the following heteroatoms as ring members: oxygen, sulfur and nitrogen, or an unsubstituted or substituted mono- or binuclear aromatic radical which, in addition to carbon atoms, can contain one to four nitrogen atoms or one or two nitrogen atoms and one oxygen or sulfur atom or one oxygen or sulfur atom as ring members;R4 is hydrogen, unsubstituted or substituted alkyl, alkenyl, alkynyl, cycloalkyl, cycloalkenyl, alkylcarbonyl or alkoxycarbonyl;  and    R5 is alkyl, alkenyl, alkynyl, cycloalkyl or cycloalkenyl, or in the case where X is NRa, additionally is hydrogen; or the salt or ester thereof. 3. The method of claim 2, wherein formula (I): n is 0 or 1;m is 0 or 1;X is 0;R1 is unsubstituted or substituted C1-C4 alkyl, C2-C4 alkenyl, or C1-C4 alkoxy;R2 is C1-C4 alkyl, C1-C4 haloalkyl, or C1-C4 alkoxy;R3 is an unsubstituted or substituted benzene;R4 is hydrogen, unsubstituted or substituted C1-C4 alkyl, C2-C4 alkenyl, or C1-C4 alkylcarbonyl;  and    R5 is C1-C4 alkyl or C2-C4 alkenyl. 4. The method of claim 1, wherein the active ingredient is methyl N-(2-{[1-(4chlorophenyl)-1H-pyrazol-3-yl]oxymethyl}phenyl)N-methoxy carbamate. 5. The method of claim 1, wherein the method further comprises mixing the pesticide with a solvent before coating the pesticide on the substrate. 6. The method of claim 5, wherein the solvent is water. 7. The method of claim 1, wherein the active ingredient chemically decomposes at temperatures within 50 deg. C. of the normal boiling point of the impurity. 8. The method of claim 1, wherein the azeotropic method is accomplished by vacuum distillation, heat, or low pressure evaporation. 9. The method of claim 1, wherein the substrate is lignin sulfonate, synthetic silicates, silica, urea, lactose, ammonium sulfate, sucrose, sodium chloride, sodium sulfate, clay, diato mite, terra alba, talc, calcium carbonate, attapulgite, water soluble polymer, or combinations thereof. 10. The method of claim 9, wherein the substrate is lignin sulfonate, silica, or a combination thereof. 11. The method of claim 1, further comprising reducing the size of the crystallized pesticide particle by an impact method. 12. The method of claim 1, wherein the crystallized pesticide has a particle size of not more than 10 mu m. 13. The method of claim 1, wherein the crystallized pesticide comprises less than 0.1 wt. % of an impurity that inhibits crystallization. 14. A method of purifying a pesticide comprising:     a) melting a pesticide having a melting point not more than about 90 deg. C., wherein the pesticide comprises at least one active ingredient and at least one impurity capable of inhibiting crystallization;b) coating the melted pesticide on a substrate to form a pesticide particle;c) substantially reducing the amount of crystallization inhibiting impurity by an azeotropic method;  and    d) crystallizing the pesticide. 15. The method of claim 14, wherein the active ingredient is methyl N-(2-{[1-(4-chlorophenyl)-1H-pyrazol-3-yl]oxymethyl}phenyl)N-methoxy carbamate. 16. The method of claim 14, wherein the method further comprises mixing the pesticide with a solvent before coating the pesticide on the substrate. 17. The method of claim 14, wherein the active ingredient chemically decomposes at temperatures within 50 deg. C. of the normal boiling point of the impurity. 18. The method of claim 14, wherein the azeotropic method is accomplished by vacuum distillation, heat, or low pressure evaporation. 19. The method of claim 14, wherein the crystallized pesticide has a particle size of not more than 10 mu m. 20. The method of claim 14, wherein the crystallized pesticide comprises less than 0.1 wt. % of an impurity that inhibits crystallization.
法律状态
(US7247175) LEGAL DETAILS FOR US2003199394  Actual or expected expiration date=2024-09-07    Legal state=ALIVE    Status=GRANTED     Event publication date=2003-03-26  Event code=US/APP  Event indicator=Pos  Event type=Examination events  Application details  Application country=US US10397765  Application date=2003-03-26  Standardized application number=2003US-10397765     Event publication date=2003-03-26  Event code=US/EXMR  Event type=Administrative notifications  USPTO Examiner Name Primary Examiner: JOHNSON, EDWARD M    Event publication date=2003-03-26  Event code=US/ART  Event type=Administrative notifications  USPTO Art Group  ART=1754     Event publication date=2003-03-26  Event code=US/ENT  Event type=Administrative notifications  Entity Status Set to Undiscounted Business Entity Status: UNDISCOUNTED    Event publication date=2003-03-26  Event code=US/AIA  Event type=Administrative notifications  First Inventor File Indicated:  AIA=No     Event publication date=2003-03-26  Event code=US/DK  Event type=Examination events  Attorney Docket Number Docket Nbr: AM200050-02    Event publication date=2003-03-26  Event code=US/CUST  Event type=Examination events  Attorney/Agent Customer Number Customer Nbr: 26474    Event publication date=2003-05-19  Event code=US/INCD  Event type=Examination events  Event type=OAO  Notice Mailed--Application Incomplete--Filing Date Assigned    Event publication date=2003-06-20  Event code=US/AS  Event type=Change of name or address  Event type=Reassignment  Assignment Owner: BASF AKTIENGESELLSCHAFT, GERMANY  Effective date of the event=2003-06-06  ASSIGNMENT OF ASSIGNORS INTEREST ASSIGNORS:FINCH, CHARLES W. FERSCH, KENNETH E. REEL/FRAME:014203/0479     Event publication date=2003-10-23  Event code=US/A1  Event type=Examination events  Application published  Publication country=US  Publication number=US2003199394  Publication stage Code=A1  Publication date=2003-10-23  Standardized publication number=US20030199394     Event publication date=2003-10-31  Event code=US/DOCK  Event indicator=Pos  Event type=Examination events  Case Docketed to Examiner    Event publication date=2004-12-07  Event code=US/CTNF  Event type=Examination events  Event type=OA  Event type=OAO  Non-Final Rejection    Event publication date=2005-01-12  Event code=US/136G  Event type=OAO  Request for Extension of Time - Granted    Event publication date=2005-05-03  Event code=US/IDS  Event type=Examination events  Event type=OAI  Information Disclosure Statement Filed    Event publication date=2005-05-03  Event code=US/CTNFR  Event type=Examination events  Event type=OAI  Response after Non-Final Action    Event publication date=2005-05-03  Event code=US/136G  Event type=OAO  Request for Extension of Time - Granted    Event publication date=2005-08-08  Event code=US/CTFR  Event type=Examination events  Event type=OA  Event type=OAO  Final Rejection    Event publication date=2005-11-10  Event code=US/NOAPLF  Event type=APL  Notice of Appeal Filed    Event publication date=2006-01-10  Event code=US/APB  Event type=APL  Event type=OAI  Appeal Brief Filed    Event publication date=2006-03-13  Event code=US/APBD  Event type=APL  Event type=OAO  Notice - Defective Appeal Brief    Event publication date=2006-03-16  Event code=US/APB  Event type=APL  Event type=OAI  Appeal Brief Filed    Event publication date=2006-04-17  Event code=US/APEA  Event type=APL  Event type=OAO  Examiner's Answer to Appeal Brief    Event publication date=2006-12-05  Event code=US/BPAIR  Event type=APL  BPAI Decision - Examiner Reversed    Event publication date=2007-03-20  Event code=US/NOAM  Event indicator=Pos  Event type=Examination events  Event type=OAO  Mail Notice of Allowance    Event publication date=2007-06-26  Event code=US/APRDY  Event indicator=Pos  Event type=Examination events  Application Is Considered Ready for Issue    Event publication date=2007-07-04  Event code=US/PAT  Event indicator=Pos  Event type=Event indicating In Force  Patented Case    Event publication date=2007-07-04  Event code=US/ISSM  Event indicator=Pos  Event type=Examination events  Event type=OAO  Event type=Restitution or restoration  Issue Notification Mailed    Event publication date=2007-07-24  Event code=US/B2  Event indicator=Pos  Event type=Event indicating In Force  Granted patent as second publication  Publication country=US  Publication number=US7247175  Publication stage Code=B2  Publication date=2007-07-24  Standardized publication number=US7247175     Event publication date=2007-07-24  Event code=US/354  Event indicator=Pos  Event type=Extension of term of duration of protection  Patent term extended under  35 U.S.C 154(b) until/for Delays (A,B,C): 196  Overlap Delays: 0  Non Overlap Delays: 587   PTO Office Delays: 0  Applicant Delays: 56  Adjustment total:  Number of days of extension=531    Event publication date=2008-04-01  Event code=US/CC  Event type=Corrections  Event type=Restitution or restoration  Certificate of Correction - Post Issue Communication    Event publication date=2010-08-03  Event code=US/NMFP  Event type=Payment or non-payment notifications  Publication of First Notice of Maintenance Fees Payable. 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专利类型码
A1B2
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