HRP20110802T1 - Kristalne modifikacije piraklostrobina - Google Patents
Kristalne modifikacije piraklostrobina Download PDFInfo
- Publication number
- HRP20110802T1 HRP20110802T1 HR20110802T HRP20110802T HRP20110802T1 HR P20110802 T1 HRP20110802 T1 HR P20110802T1 HR 20110802 T HR20110802 T HR 20110802T HR P20110802 T HRP20110802 T HR P20110802T HR P20110802 T1 HRP20110802 T1 HR P20110802T1
- Authority
- HR
- Croatia
- Prior art keywords
- pyraclostrobin
- modification
- crystallization
- organic solvent
- volume
- Prior art date
Links
- 239000005869 Pyraclostrobin Substances 0.000 title claims abstract 23
- HZRSNVGNWUDEFX-UHFFFAOYSA-N pyraclostrobin Chemical compound COC(=O)N(OC)C1=CC=CC=C1COC1=NN(C=2C=CC(Cl)=CC=2)C=C1 HZRSNVGNWUDEFX-UHFFFAOYSA-N 0.000 title claims abstract 23
- 230000004048 modification Effects 0.000 title claims abstract 15
- 238000012986 modification Methods 0.000 title claims abstract 15
- 238000000034 method Methods 0.000 claims 11
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims 6
- 239000013078 crystal Substances 0.000 claims 6
- 238000002425 crystallisation Methods 0.000 claims 6
- 230000008025 crystallization Effects 0.000 claims 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims 5
- 239000003960 organic solvent Substances 0.000 claims 4
- 239000003791 organic solvent mixture Substances 0.000 claims 4
- 239000000725 suspension Substances 0.000 claims 4
- 238000010899 nucleation Methods 0.000 claims 3
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims 2
- 239000002904 solvent Substances 0.000 claims 2
- 241000233866 Fungi Species 0.000 claims 1
- 239000000969 carrier Substances 0.000 claims 1
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 239000012141 concentrate Substances 0.000 claims 1
- 238000004090 dissolution Methods 0.000 claims 1
- 238000002844 melting Methods 0.000 claims 1
- 230000008018 melting Effects 0.000 claims 1
- 238000002156 mixing Methods 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 230000003032 phytopathogenic effect Effects 0.000 claims 1
- 239000000843 powder Substances 0.000 claims 1
- 239000011814 protection agent Substances 0.000 claims 1
- 230000005855 radiation Effects 0.000 claims 1
- 239000000126 substance Substances 0.000 claims 1
- 238000000634 powder X-ray diffraction Methods 0.000 abstract 1
Classifications
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
- A01N47/08—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having one or more single bonds to nitrogen atoms
- A01N47/10—Carbamic acid derivatives, i.e. containing the group —O—CO—N<; Thio analogues thereof
- A01N47/24—Carbamic acid derivatives, i.e. containing the group —O—CO—N<; Thio analogues thereof containing the groups, or; Thio analogues thereof
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D231/00—Heterocyclic compounds containing 1,2-diazole or hydrogenated 1,2-diazole rings
- C07D231/02—Heterocyclic compounds containing 1,2-diazole or hydrogenated 1,2-diazole rings not condensed with other rings
- C07D231/10—Heterocyclic compounds containing 1,2-diazole or hydrogenated 1,2-diazole rings not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members
- C07D231/14—Heterocyclic compounds containing 1,2-diazole or hydrogenated 1,2-diazole rings not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D231/18—One oxygen or sulfur atom
- C07D231/20—One oxygen atom attached in position 3 or 5
- C07D231/22—One oxygen atom attached in position 3 or 5 with aryl radicals attached to ring nitrogen atoms
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical & Material Sciences (AREA)
- Environmental Sciences (AREA)
- Agronomy & Crop Science (AREA)
- Engineering & Computer Science (AREA)
- Dentistry (AREA)
- General Health & Medical Sciences (AREA)
- Wood Science & Technology (AREA)
- Zoology (AREA)
- Plant Pathology (AREA)
- Pest Control & Pesticides (AREA)
- Health & Medical Sciences (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
- Saccharide Compounds (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Medicines Containing Plant Substances (AREA)
- Heterocyclic Carbon Compounds Containing A Hetero Ring Having Oxygen Or Sulfur (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
- Plural Heterocyclic Compounds (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
Kristalna modifikacija IV piraklostrobina, naznačena time, što na difraktogramu dobijenom primjenom rentgenskog zračenja na prahu na 25°C pokazuje najmanje tri slijedeće refleksije: d = 6,02 ± 0,01 ? d = 4,78 ± 0,01 ? d = 4,01 ± 0,01 ? d = 3,55 ± 0,01 ? d = 3,01 ± 0,01 ?. Patent sadrži još 16 patentnih zahtjeva.
Claims (17)
1. Kristalna modifikacija IV piraklostrobina, naznačena time, što na difraktogramu dobijenom primjenom rentgenskog zračenja na prahu na pokazuje najmanje tri slijedeće refleksije:
d = 6,02 ± 0,01 Å
d = 4,78 ± 0,01 Å
d = 4,01 ± 0,01 Å
d = 3,55 ± 0,01 Å
d = 3,01 ± 0,01 Å.
2. Kristalna modifikacija IV prema zahtjevu 1, naznačena time, što je točka topljenja u opsegu od 62 do .
3. Kristalna modifikacija IV prema zahtjevu 1, naznačena time, što je sadržaj piraklostrobina od najmanje 98 tež. %.
4. Postupak za dobijanje kristalne modifikacije IV piraklostrobina prema jednom od prethodnih zahtjeva, naznačen time, što sadrži:
i) otapanje piraklostrobina koji ima drugačiji oblik od modifikacije IV u organskom otapalu ili smjesi otapala, pri čemu organsko otapalo ili smjesa otapala sadrži najmanje 70 vol. % najmanje jednog otapala koje se potpuno miješa sa vodom L1 i eventualno do 30 vol. % vode; i
ii) vršenje kristalizacije piraklostrobina u toku vremenskog perioda od najmanje 10 h i/ili u prisustvu kristala za zasijavanje modifikacije IV.
5. Postupak prema zahtjevu 4, naznačen time, što se otapanje piraklostrobina vrši na temperaturi iznad .
6. Postupak prema zahtjevu 5, naznačen time, što se zbog kristalizacije piraklostrobina otopina hladi.
7. Postupak prema jednom od zahtjeva 4 do 6, naznačen time, što se kristalizacija piraklostrobina vrši dodavanjem vode otopini piraklostrobina.
8. Postupak prema jednom od zahtjeva 4 do 7, pri čemu se u toku kristalizacije piraklostrobina ili prije nje dodaju kristali za zasijavanje modifikacije IV.
9. Postupak prema jednom od zahtjeva 4 do 8, naznačen time, što je organsko otapalo koje se potpuno miješa sa vodom L1 izabrano između C1-C4-alkanola, acetona i butanona.
10. Postupak prema zahtjevu 9, naznačen time, što se u koraku i) za otapanje piraklostrobina upotrebljavaju metanol, etanol ili smjesa otapala koja sadrži najmanje 70 vol. % metanola i/ili etanola.
11. Postupak prema jednom od zahtjeva 4 do 10, naznačen time, što se poslije kristalizacije dijela količine piraklostrobina sadržane u otopini, dodaje voda radi završetka kristalizacije piraklostrobina.
12. Postupak za dobijanje kristalne modifikacije IV piraklostrobina prema jednom od zahtjeva 1 do 3, naznačen time, što sadrži:
i) dobijanje suspenzije piraklostrobina koji ima drugačiji oblik od modifikacije IV piraklostrobina u jednom organskom otapalu;
ii) eventualno dodavanje kristala za zasijavanje modifikacije IV suspenziji;
iii) miješanje suspenzije sve dok najmanje 90 % piraklostrobina sadržanog u njoj ne bude u obliku modifikacije IV.
13. Postupak prema zahtjevu 12, naznačen time, što organsko otapalo koje se upotrebljava u koraku i) za suspendiranje piraklostrobina sadrži najmanje 50 vol. % najmanje jednog C1-C4-alkanola.
14. Postupak prema zahtjevu 13, pri čemu organsko otapalo koje se upotrebljava u koraku i) za suspendiranje piraklostrobina sadrži najmanje 70 vol. % metanola, izopropanola i/ili etanola.
15. Sredstvo za zaštitu bilja koje sadrži piraklostrobin u obliku modifikacije IV prema jednom od zahtjeva 1 do 3, naznačeno time, što sadrži i uobičajene nosače i/ili pomoćne materije.
16. Sredstvo prema zahtjevu 15, naznačeno time, što je u obliku vodenog koncentrata za suspenziju.
17. Primjena piraklostrobina u obliku modifikacije IV prema jednom od zahtjeva 1 do 3, naznačena time, što se koristi za kontrolu fitopatogenih gljiva.
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE102005028493 | 2005-06-20 | ||
PCT/EP2006/005869 WO2006136357A2 (de) | 2005-06-20 | 2006-06-19 | Kristalline modifikationen des pyraclostrobins |
Publications (1)
Publication Number | Publication Date |
---|---|
HRP20110802T1 true HRP20110802T1 (hr) | 2011-11-30 |
Family
ID=37570793
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
HR20110802T HRP20110802T1 (hr) | 2005-06-20 | 2011-11-02 | Kristalne modifikacije piraklostrobina |
Country Status (34)
Country | Link |
---|---|
US (2) | US7816392B2 (hr) |
EP (2) | EP1937071B1 (hr) |
JP (2) | JP4997231B2 (hr) |
KR (1) | KR101323051B1 (hr) |
CN (1) | CN101203136B (hr) |
AP (1) | AP2443A (hr) |
AR (2) | AR054777A1 (hr) |
AT (1) | ATE521238T1 (hr) |
AU (1) | AU2006261191B2 (hr) |
BR (1) | BRPI0612246B1 (hr) |
CA (1) | CA2612075C (hr) |
CR (1) | CR9569A (hr) |
CY (1) | CY1112653T1 (hr) |
DK (1) | DK1937071T3 (hr) |
EA (1) | EA012454B1 (hr) |
EC (2) | ECSP078032A (hr) |
ES (1) | ES2371270T3 (hr) |
GT (1) | GT200600264A (hr) |
HR (1) | HRP20110802T1 (hr) |
IL (2) | IL188240A0 (hr) |
MA (1) | MA29627B1 (hr) |
ME (1) | ME01961B (hr) |
MX (1) | MX2007016271A (hr) |
NZ (1) | NZ564023A (hr) |
PE (1) | PE20070090A1 (hr) |
PL (1) | PL1937071T3 (hr) |
PT (1) | PT1937071E (hr) |
RS (1) | RS51954B (hr) |
SI (1) | SI1937071T1 (hr) |
TW (1) | TWI393707B (hr) |
UA (1) | UA89830C2 (hr) |
UY (1) | UY29611A1 (hr) |
WO (1) | WO2006136357A2 (hr) |
ZA (2) | ZA200800504B (hr) |
Families Citing this family (28)
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---|---|---|---|---|
TW200901889A (en) * | 2007-02-09 | 2009-01-16 | Basf Se | Crystalline complexes of agriculturally active organic compounds |
EP2309847A2 (de) * | 2008-07-24 | 2011-04-20 | Basf Se | Öl-in-wasser emulsion umfassend lösungsmittel, wasser, tensid und pestizid |
WO2010015578A1 (en) * | 2008-08-04 | 2010-02-11 | Basf Se | Method for controlling fungal diseases in legumes |
UA106213C2 (ru) * | 2008-10-10 | 2014-08-11 | Басф Се | Жидкие препараты для защиты растений, содержащие пираклостробин |
TW201018400A (en) | 2008-10-10 | 2010-05-16 | Basf Se | Liquid aqueous plant protection formulations |
WO2011006896A2 (en) * | 2009-07-14 | 2011-01-20 | Basf Se | A process for preparing an aqueous suspension of an organic pesticide compound |
KR20120115492A (ko) | 2009-11-06 | 2012-10-18 | 바스프 에스이 | 4―히드록시 벤조산 및 선택된 살충제의 결정질 복합체 |
CN103237451A (zh) * | 2010-12-08 | 2013-08-07 | 巴斯夫欧洲公司 | 杀真菌混合物 |
CN102177902A (zh) * | 2011-03-19 | 2011-09-14 | 陕西汤普森生物科技有限公司 | 一种含有吡唑醚菌酯的增效杀菌组合物 |
CN102177912A (zh) * | 2011-03-23 | 2011-09-14 | 陕西汤普森生物科技有限公司 | 一种含有吡唑醚菌酯的农药组合物 |
CN102100234B (zh) * | 2011-03-23 | 2014-03-05 | 陕西汤普森生物科技有限公司 | 一种含吡唑醚菌酯与氨基甲酸酯类的杀菌组合物 |
CN102273474A (zh) * | 2011-08-22 | 2011-12-14 | 吴元林 | 一种含春雷霉素与吡唑醚菌酯的杀菌剂组合物及其应用 |
CN102399190A (zh) * | 2011-12-20 | 2012-04-04 | 河南中医学院 | 一种经济型合成吡唑醚菌酯及其方法 |
CN102428953A (zh) * | 2012-01-14 | 2012-05-02 | 陕西美邦农药有限公司 | 一种含硅噻菌胺与甲氧基丙烯酸酯类化合物的杀菌组合物 |
CN102669137A (zh) * | 2012-05-17 | 2012-09-19 | 广东中迅农科股份有限公司 | 一种杀菌药肥颗粒剂 |
CN102805090A (zh) * | 2012-07-11 | 2012-12-05 | 广东中迅农科股份有限公司 | 一种吡唑醚菌酯水悬浮剂及其制备方法 |
US9770030B2 (en) * | 2013-04-03 | 2017-09-26 | Fmc Corporation | Suspoemulsion of fomesafen and fluthiacet-methyl |
CN104365590B (zh) * | 2014-12-01 | 2016-03-30 | 山东省联合农药工业有限公司 | 一种连续化的吡唑醚菌酯悬浮剂制备方法 |
CN104872160A (zh) * | 2015-05-14 | 2015-09-02 | 京博农化科技股份有限公司 | 一种吡唑醚菌酯制剂及其制备方法 |
CA2994399C (en) | 2015-08-10 | 2023-10-17 | Basf Se | A process for preparing crystalline methyl n-[2-[[[1-(4-chlorophen yl)-1h-pyrazol-3-yl]oxy]methyl]phenyl]-n-methoxycarbamate |
GB2552694B (en) * | 2016-08-04 | 2020-03-04 | Rotam Agrochem Int Co Ltd | A Synergistic fungicidal composition and use thereof |
CN106928144A (zh) * | 2017-03-16 | 2017-07-07 | 上海晓明检测技术服务有限公司 | 一种高纯度吡唑醚菌酯标准品的制备方法 |
CN106866533B (zh) * | 2017-03-28 | 2022-03-11 | 天津大学 | 吡唑醚菌酯晶型及制备方法 |
CN106977459B (zh) * | 2017-03-28 | 2019-11-29 | 天津大学 | 一种提高吡唑醚菌酯堆密度和流动性的结晶方法 |
CN107021927B (zh) * | 2017-03-28 | 2020-05-29 | 天津大学 | 一种吡唑醚菌酯晶型及其制备方法 |
CN108117521A (zh) * | 2018-03-05 | 2018-06-05 | 安徽国星生物化学有限公司 | 一种吡唑醚菌酯的反向重结晶方法 |
CN110041258A (zh) * | 2019-04-26 | 2019-07-23 | 永农生物科学有限公司 | 一种吡唑醚菌酯的混合晶型及其制备方法 |
CN110590672A (zh) * | 2019-09-09 | 2019-12-20 | 海利尔药业集团股份有限公司 | 一种吡唑醚菌酯ⅱ型晶型的制备方法 |
Family Cites Families (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE4423612A1 (de) | 1994-07-06 | 1996-01-11 | Basf Ag | 2-[(Dihydro)pyrazolyl-3'-oxymethylen]-anilide, Verfahren zu ihrer Herstelung und ihre Verwendung |
TW460476B (en) | 1997-04-14 | 2001-10-21 | American Cyanamid Co | Fungicidal trifluoromethylalkylamino-triazolopyrimidines |
DK1054888T3 (da) | 1998-02-11 | 2004-04-05 | Basf Ag | Fungicide 7-alkyl-triazolpyrimidiner |
WO2003004465A2 (de) | 2001-07-05 | 2003-01-16 | Basf Aktiengesellschaft | Fungizide triazolopyrimidine, verfahren zu ihrer herstellung und ihre verwendung zur bekämpfung von schadpilzen sowie sie enthaltende mittel |
IL163867A0 (en) * | 2002-03-28 | 2005-12-18 | Basf Ag | Method of purifying a pesticide |
DE10233171A1 (de) * | 2002-07-22 | 2004-02-12 | Bayer Cropscience Ag | Kristallmodifikation II des 2-[2-(Chlor-cyclopropyl)-3-(2-chlorphenyl)-2-hydroxy-propyl]-2,4dihydro-3H-1,2,4-triazol-3-thions |
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2006
- 2006-06-15 AR ARP060102535A patent/AR054777A1/es not_active Application Discontinuation
- 2006-06-16 PE PE2006000681A patent/PE20070090A1/es active IP Right Grant
- 2006-06-19 BR BRPI0612246-9A patent/BRPI0612246B1/pt active IP Right Grant
- 2006-06-19 CN CN2006800222049A patent/CN101203136B/zh active Active
- 2006-06-19 AP AP2007004294A patent/AP2443A/xx active
- 2006-06-19 NZ NZ564023A patent/NZ564023A/en unknown
- 2006-06-19 EP EP06762088A patent/EP1937071B1/de active Active
- 2006-06-19 DK DK06762088.0T patent/DK1937071T3/da active
- 2006-06-19 ME MEP-2011-475A patent/ME01961B/me unknown
- 2006-06-19 UA UAA200800568A patent/UA89830C2/ru unknown
- 2006-06-19 MX MX2007016271A patent/MX2007016271A/es active IP Right Grant
- 2006-06-19 RS RS20110475A patent/RS51954B/en unknown
- 2006-06-19 SI SI200631163T patent/SI1937071T1/sl unknown
- 2006-06-19 US US11/917,976 patent/US7816392B2/en active Active
- 2006-06-19 ES ES06762088T patent/ES2371270T3/es active Active
- 2006-06-19 PL PL06762088T patent/PL1937071T3/pl unknown
- 2006-06-19 EP EP10175103A patent/EP2305033A1/de not_active Withdrawn
- 2006-06-19 WO PCT/EP2006/005869 patent/WO2006136357A2/de active Application Filing
- 2006-06-19 JP JP2008516250A patent/JP4997231B2/ja active Active
- 2006-06-19 EA EA200702586A patent/EA012454B1/ru not_active IP Right Cessation
- 2006-06-19 AT AT06762088T patent/ATE521238T1/de active
- 2006-06-19 KR KR1020077029557A patent/KR101323051B1/ko active IP Right Review Request
- 2006-06-19 CA CA2612075A patent/CA2612075C/en active Active
- 2006-06-19 PT PT06762088T patent/PT1937071E/pt unknown
- 2006-06-19 AU AU2006261191A patent/AU2006261191B2/en active Active
- 2006-06-19 GT GT200600264A patent/GT200600264A/es unknown
- 2006-06-20 UY UY29611A patent/UY29611A1/es not_active Application Discontinuation
- 2006-06-20 TW TW095122073A patent/TWI393707B/zh active
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2007
- 2007-12-06 CR CR9569A patent/CR9569A/es unknown
- 2007-12-18 EC EC2007008032A patent/ECSP078032A/es unknown
- 2007-12-19 IL IL188240A patent/IL188240A0/en active IP Right Grant
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2008
- 2008-01-14 MA MA30569A patent/MA29627B1/fr unknown
- 2008-01-17 ZA ZA2008/00504A patent/ZA200800504B/en unknown
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2010
- 2010-09-16 US US12/883,216 patent/US8404734B2/en active Active
- 2010-12-06 ZA ZA2010/08744A patent/ZA201008744B/en unknown
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2011
- 2011-09-07 IL IL215015A patent/IL215015A0/en unknown
- 2011-10-19 JP JP2011229798A patent/JP2012067107A/ja not_active Withdrawn
- 2011-11-02 HR HR20110802T patent/HRP20110802T1/hr unknown
- 2011-11-22 CY CY20111101131T patent/CY1112653T1/el unknown
- 2011-12-22 EC EC2011008032A patent/ECSP11008032A/es unknown
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2014
- 2014-07-04 AR ARP140102502A patent/AR096819A2/es not_active Application Discontinuation
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