HRP20131153T1 - Novi kristalni oblik 3-(difluorometil)-1-metil-n-(3', 4', 5'-trifluoro[1,1'-bifenil]-2-il)-1h-pirazol-4-karboksamida - Google Patents
Novi kristalni oblik 3-(difluorometil)-1-metil-n-(3', 4', 5'-trifluoro[1,1'-bifenil]-2-il)-1h-pirazol-4-karboksamida Download PDFInfo
- Publication number
- HRP20131153T1 HRP20131153T1 HRP20131153AT HRP20131153T HRP20131153T1 HR P20131153 T1 HRP20131153 T1 HR P20131153T1 HR P20131153A T HRP20131153A T HR P20131153AT HR P20131153 T HRP20131153 T HR P20131153T HR P20131153 T1 HRP20131153 T1 HR P20131153T1
- Authority
- HR
- Croatia
- Prior art keywords
- biphenyl
- methyl
- carboxamide
- difluoromethyl
- trifluoro
- Prior art date
Links
- SXSGXWCSHSVPGB-UHFFFAOYSA-N fluxapyroxad Chemical compound FC(F)C1=NN(C)C=C1C(=O)NC1=CC=CC=C1C1=CC(F)=C(F)C(F)=C1 SXSGXWCSHSVPGB-UHFFFAOYSA-N 0.000 claims 8
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims 6
- 239000013078 crystal Substances 0.000 claims 5
- 239000011814 protection agent Substances 0.000 claims 5
- 238000000034 method Methods 0.000 claims 4
- 238000004519 manufacturing process Methods 0.000 claims 3
- 239000000203 mixture Substances 0.000 claims 3
- 239000003849 aromatic solvent Substances 0.000 claims 2
- 239000012141 concentrate Substances 0.000 claims 2
- 150000004292 cyclic ethers Chemical class 0.000 claims 2
- 239000007788 liquid Substances 0.000 claims 2
- 239000003960 organic solvent Substances 0.000 claims 2
- 238000002360 preparation method Methods 0.000 claims 2
- 238000000926 separation method Methods 0.000 claims 2
- 239000002904 solvent Substances 0.000 claims 2
- 239000000725 suspension Substances 0.000 claims 2
- 238000004566 IR spectroscopy Methods 0.000 claims 1
- 238000010521 absorption reaction Methods 0.000 claims 1
- 239000000654 additive Substances 0.000 claims 1
- 239000000010 aprotic solvent Substances 0.000 claims 1
- 150000001875 compounds Chemical class 0.000 claims 1
- 238000001816 cooling Methods 0.000 claims 1
- 238000010586 diagram Methods 0.000 claims 1
- 238000009472 formulation Methods 0.000 claims 1
- 239000008187 granular material Substances 0.000 claims 1
- 238000010438 heat treatment Methods 0.000 claims 1
- 239000000843 powder Substances 0.000 claims 1
- 238000000634 powder X-ray diffraction Methods 0.000 claims 1
- 230000005855 radiation Effects 0.000 claims 1
Classifications
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Plural Heterocyclic Compounds (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Claims (12)
1. Kristalni oblik B 3-(difluorometil)-1-metil-N -(3',4',5'-trifluor[1,1'-bifenil]-2-il)-1H-pirazol-4-karboksamida, naznačen time što u dijagramu rendgenske difrakcije praha na 25°C i Cu-Kαzračenju pokazuje najmanje 3 od slijedećih refleksija, navedenih kao 2θ vrijednosti: 6.2 ± 0.2°, 9.2 ± 0.2°, 13.2 ± 0.2°, 14.9 ± 0.2°, 17.7 ± 0.2°, 18.6 ± 0.2°, 23.1 ± 0.2°, 27.6° ± 0.2°, 30.5 ± 0.2°.
2. Kristalni oblik B 3-(difluorometil)-1-metil-N -(3',4',5'-trifluor[1,1'-bifenil]-2-il)-1H-pirazol-4-karboksamida, naznačen time što sadrži karakteristične apsorpcione trake prema Fourier-ovoj transformisanoj infracrvenoj spektroskopiji na valnim dužinama 3256 cm-1i 1639 cm-1.
3. Kristalni oblik B prema patentnom zahtjevu 1 sa sadržajem 3-(difluorometil)-1-metil-N -(3',4',5'-trifluor[1,1'-bifenil]-2-il)-1H-pirazol-4-karboksamidaod najmanje 94 tež.%.
4. 3-(Difluorometil)-1-metil-N-(3',4',5'-trifluor[1,1'-bifenil]-2-il)-1H-pirazol-4-karboksamid naznačen time što se sastoji od najmanje 90 tež.% kristalnog oblika B prema patentnom zahtjevu 1.
5. Postupak za proizvodnju kristalnog oblika B prema patentnom zahtjevu 1 ili 2, naznačen time što sadrži:
pripremu otopine3-(difluorometil)-1-metil-N-(3',4',5'-trifluor[1,1'-bifenil]-2-il)-1H-pirazol-4-karboksamidau organskom otapalu koje je izabrano od metanola, etanola, 2-propanola, cikličnih etera, octene kiseline, aporotonskih otapala i aromatičnih otapala, na 50 do 130°C,
hlađenje otopine na stopi od između 20°C/čas i 0,1°C/čas do temperature između 70°C i (-20)°C, i
odvajanje oblika B iz ishodne tekućine.
6. Postupak za proizvodnju kristalnog oblika B prema patentnom zahtjevu 1 ili 2, naznačen time što sadrži
pripremu otopine3-(difluorometil)-1-metil-N-(3',4',5'-trifluor[1,1'-bifenil]-2-il)-1H-pirazol-4-karboksamidau organskom otapalu koje je izabrano od metanola, etanola, 2-propanola, cikličnih etera, octene kiseline, aprotonskih otapala i aromatičnih otapala, na 50 do 130°C,
dodavanje otapala za smanjenje otopljivosti u otopinu u toku razdoblja od 40 minuta do 2.5 sata,
odvajanje oblika B iz ishodne tekućine.
7. Postupak za proizvodnju kristalnog oblika B prema patentnom zahtjevu 1 ili 2, koji sadrži zagrijavanje amorfnog spoja, njegovog kristalnog oblika A, smjese amorfnog oblika sa oblikom A ili smjese oblika B sa amorfnim oblikom ili oblikom A na 80°C do 154°C, pri čemu je kristalni oblik A naznačen monokliničkim kristalnim sustavom sa prostornom grupom P2(1)/C.
8. Sredstvo za zaštitu biljaka naznačeno time što sadrži 3-(difluorometil)-1-metil-N-(3',4',5'-trifluor[1,1'-bifenil]-2-il)-1H-pirazol-4-karboksamidkoji se sastoji od najmanje 90 tež.% kristalnog oblika B prema patentnom zahtjevu1, i jedan ili više aditiva normalnih za formulaciju sredstava za zaštitu biljaka.
9. Sredstvo za zaštitu biljaka prema patentnom zahtjevu 8 u obliku vodenog koncentrata za suspenziju.
10. Sredstvo za zaštitu biljaka prema patentnom zahtjevu 8 u obliku nevodenog koncentrata za suspenziju.
11. Sredstvo za zaštitu biljaka prema patentnom zahtjevu 8 u obliku praška ili granula raspršivih u vodi.
12. Postupak za borbu protiv rasta neželjenih biljaka, naznačen time što se 3-(difluorometil)-1-metil-N-(3',4',5'-trifluor[1,1'-bifenil]-2-il)-1H-pirazol-4-karboksamidkoji se sastoji od najmanje 90 tež.% kristalnog oblika B prema patentnom zahtjevu 1 ili 2 koristi na biljkama, njihovom staništu i/ili sjemenju.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| EP07112393 | 2007-07-12 | ||
| PCT/EP2008/058785 WO2009007344A1 (en) | 2007-07-12 | 2008-07-07 | Novel crystalline form of 3-(difluormethyl)-1-methyl-n -(3',4',5'-trifluor[1,1'-biphenyl]-2-yl)-1h-pyrazol-4-carboxamide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| HRP20131153T1 true HRP20131153T1 (hr) | 2014-01-03 |
Family
ID=39008245
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| HRP20131153AT HRP20131153T1 (hr) | 2007-07-12 | 2013-12-03 | Novi kristalni oblik 3-(difluorometil)-1-metil-n-(3', 4', 5'-trifluoro[1,1'-bifenil]-2-il)-1h-pirazol-4-karboksamida |
Country Status (29)
| Country | Link |
|---|---|
| US (1) | US8101780B2 (hr) |
| EP (1) | EP2176229B1 (hr) |
| JP (1) | JP5442604B2 (hr) |
| KR (1) | KR20100043069A (hr) |
| CN (1) | CN101743225B (hr) |
| AR (1) | AR068079A1 (hr) |
| BR (1) | BRPI0814690B1 (hr) |
| CA (1) | CA2692421C (hr) |
| CL (1) | CL2008002045A1 (hr) |
| CR (1) | CR11170A (hr) |
| DK (1) | DK2176229T3 (hr) |
| EA (1) | EA016798B1 (hr) |
| EC (1) | ECSP109938A (hr) |
| ES (1) | ES2436292T3 (hr) |
| HR (1) | HRP20131153T1 (hr) |
| IL (1) | IL202654A (hr) |
| MA (1) | MA31603B1 (hr) |
| MX (1) | MX2009013808A (hr) |
| NZ (1) | NZ583201A (hr) |
| PE (1) | PE20090440A1 (hr) |
| PL (1) | PL2176229T3 (hr) |
| PT (1) | PT2176229E (hr) |
| RS (1) | RS53057B (hr) |
| SI (1) | SI2176229T1 (hr) |
| TW (1) | TWI469735B (hr) |
| UA (1) | UA99919C2 (hr) |
| UY (1) | UY31223A1 (hr) |
| WO (1) | WO2009007344A1 (hr) |
| ZA (1) | ZA201000971B (hr) |
Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012066122A1 (en) | 2010-11-18 | 2012-05-24 | Syngenta Participations Ag | 2 - (pyridin- 2 -yl) -quinazoline derivatives and their use as microbicides |
| WO2013011010A1 (en) | 2011-07-19 | 2013-01-24 | Syngenta Participations Ag | Fungizide mixtures |
| GB201202393D0 (en) * | 2012-02-09 | 2012-03-28 | Syngenta Ltd | Polymorphs |
| JP2013166724A (ja) * | 2012-02-16 | 2013-08-29 | Sumitomo Chemical Co Ltd | フルミオキサジンの結晶形 |
| WO2013132006A1 (de) | 2012-03-07 | 2013-09-12 | Friedrich-Alexander-Universität Erlangen-Nürnberg | Verfahren zur synthese von aminobiphenylen unter verwendung von arylhydrazinen |
| US9598826B2 (en) | 2012-10-30 | 2017-03-21 | Capstan Ag Systems, Inc. | Paint spraying system |
| TWI652012B (zh) * | 2013-05-20 | 2019-03-01 | 杜邦股份有限公司 | 殺真菌吡唑的固態形式 |
| WO2022072650A1 (en) | 2020-10-01 | 2022-04-07 | Corteva Agriscience Llc | Polymorphs of compounds having pesticidal activity |
| JP7419276B2 (ja) | 2021-01-12 | 2024-01-22 | 株式会社クボタ | 作業機 |
| CN113134426B (zh) * | 2021-04-01 | 2023-03-31 | 佛山市南海华昊华丰淀粉有限公司 | 一种通过离心机且以水汽加热的变性淀粉粉化设备 |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102005007160A1 (de) * | 2005-02-16 | 2006-08-24 | Basf Ag | Pyrazolcarbonsäureanilide, Verfahren zu ihrer Herstellung und sie enthaltende Mittel zur Bekämpfung von Schadpilzen |
| CA2617503C (en) * | 2005-08-05 | 2014-07-15 | Basf Aktiengesellschaft | Fungicidal mixtures containing substituted 1-methyl pyrazol-4-yl carboxylic acid |
| ATE455105T1 (de) * | 2006-11-03 | 2010-01-15 | Basf Se | Verfahren zur herstellung von difluormethylpyrazolylcarboxylaten |
| KR101517254B1 (ko) * | 2007-06-01 | 2015-04-30 | 바스프 에스이 | Ｎ-치환된 (3-디할로메틸-1-메틸-피라졸-4-일)카르복사미드의 제조 방법 |
-
2008
- 2008-07-07 RS RS20130526A patent/RS53057B/en unknown
- 2008-07-07 WO PCT/EP2008/058785 patent/WO2009007344A1/en active Application Filing
- 2008-07-07 CA CA2692421A patent/CA2692421C/en active Active
- 2008-07-07 UA UAA201001370A patent/UA99919C2/ru unknown
- 2008-07-07 EA EA201000095A patent/EA016798B1/ru not_active IP Right Cessation
- 2008-07-07 ES ES08785959T patent/ES2436292T3/es active Active
- 2008-07-07 BR BRPI0814690-0A patent/BRPI0814690B1/pt active IP Right Grant
- 2008-07-07 PL PL08785959T patent/PL2176229T3/pl unknown
- 2008-07-07 DK DK08785959.1T patent/DK2176229T3/da active
- 2008-07-07 MX MX2009013808A patent/MX2009013808A/es active IP Right Grant
- 2008-07-07 PT PT87859591T patent/PT2176229E/pt unknown
- 2008-07-07 EP EP08785959.1A patent/EP2176229B1/en active Active
- 2008-07-07 NZ NZ583201A patent/NZ583201A/en unknown
- 2008-07-07 SI SI200831113T patent/SI2176229T1/sl unknown
- 2008-07-07 KR KR1020107003087A patent/KR20100043069A/ko not_active Application Discontinuation
- 2008-07-07 CN CN2008800243468A patent/CN101743225B/zh active Active
- 2008-07-07 JP JP2010515484A patent/JP5442604B2/ja active Active
- 2008-07-07 US US12/668,242 patent/US8101780B2/en active Active
- 2008-07-11 UY UY31223A patent/UY31223A1/es unknown
- 2008-07-11 CL CL2008002045A patent/CL2008002045A1/es unknown
- 2008-07-11 TW TW97126520A patent/TWI469735B/zh not_active IP Right Cessation
- 2008-07-11 PE PE2008001163A patent/PE20090440A1/es not_active Application Discontinuation
- 2008-07-11 AR ARP080103005A patent/AR068079A1/es unknown
-
2009
- 2009-12-10 IL IL202654A patent/IL202654A/en not_active IP Right Cessation
- 2009-12-16 CR CR11170A patent/CR11170A/es unknown
-
2010
- 2010-02-04 EC EC2010009938A patent/ECSP109938A/es unknown
- 2010-02-09 MA MA32606A patent/MA31603B1/fr unknown
- 2010-02-10 ZA ZA2010/00971A patent/ZA201000971B/en unknown
-
2013
- 2013-12-03 HR HRP20131153AT patent/HRP20131153T1/hr unknown
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