专利号:US-2015239796-A1 优先权日:2014-02-19 标题:One pot synthesis of 18f labeledtrifluoromethylated compounds with difluoro(iodo)methane 发明人:RüHL THOMAS; RISS PATRICK; RAFIQUE WAQAS 权利人:UNIV OSLO 摘要:The present invention relates to compositions and methods for the synthesis of 18 F labeled compounds. In particular, the present invention relates to a copper (I) mediated one pot method for 18 F-trifluoromethylation of aromatic- or heteroaromatic halides with difluoro(iodo)methane (e.g., for use at PET imaging agents).
专利号:US-8129521-B2 优先权日:2005-12-14 标 题 :One pot synthesis of tetrazole derivatives of rapamycin 发明人:DHAON MADHUP K; HSIAO CHI-NUNG; PATEL SUBHASH R; BONK PETER J; CHEMBURKAR SANJAY R; CHEN YONG Y 权利人:DHAON MADHUP K; HSIAO CHI-NUNG; PATEL SUBHASH R; BONK PETER J; CHEMBURKAR SANJAY R; CHEN YONG Y; ABBOTT LAB 摘要:A single-step, one-pot process to obtain zotarolimus and other rapamycin derivatives on large scale is presented, which improves currently available synthesis schemes. In one embodiment, dried rapamycin is dissolved in isopropylacetate (IPAc). The solution is cooled, and 2,6-Lutidine is added, followed slowly adding triflic anhydride at −30° C. Salts are then removed by filtration. Tetrazole, followed by a tert-base diisopropylethylamine (DIEA) is added to the triflate solution. After incubation at room temperature, the product is concentrated and purified by a silica gel column using THF/heptane as eluant. The fractions containing the product are collected, concentrated, and purified again using an acetone/heptane column. The product containing fractions are concentrated. The product is dissolved in t-BME and precipitated with heptane. The solids are dissolved in acetone, treated with butylated-hydroxy toluene (BHT), and the solution concentrated. The process is repeated twice with acetone to remove solvents. At least one stabilizing agent is added, such as BHT at 0.5% before drying.
专利号:WO-2011092618-A1 优先权日:2010-01-28 标题 :Method for the preparation of fluazinam 发明人:PASTORIO ANDREA; MORA CLAUDIA 权利人:FINCHIMICA SRL; PASTORIO ANDREA; MORA CLAUDIA 摘要:A method for the synthesis of 3-chloro, N- (3-chloro-5- trifluoromethyl-2-pyridyl), α, α, α-trif luoro, 2,6-dinitro- p-toluidine (Fluazinam) comprises an amination reaction of a pyridine, to obtain 2-amino, 3-chloro, 5- trif luoromethylpyridine, the addition of a strong base to the 2-amino, 3-chloro, 5-trif luoromethylpyridine, and a formation reaction of Fluazinam by coupling of the 2- amino-3-chloro-5-trif luoromethylpyridine with the 2,4- dichloro, 3,5-dinitro, benzotrif luoride. The amination reaction is conducted with anhydrous ammonia in an organic solvent. Furthermore, the coupling reaction as above takes place directly in the solution of Pyridine 2 coming from the amination step.
专利号:WO-2025056767-A1 优先权日:2023-09-15 标题 :Process for the preparation of enantiomerically enriched aliphatic amines 发明人:BOU HAMDAN FARHAN; GODINEAU EDOUARD; SMEJKAL TOMAS; DUMEUNIER RAPHAEL; BOUSSEMGHOUNE MOHAMED ABDELOUAHAB; BLUM MATHIAS 权利人:SYNGENTA CROP PROTECTION AG 摘要:The present invention relates to a process for the preparation of enantiomerically enriched cyclobutylamines of formula (I) from α-tertiary cyclobutanones and reacting said enantiomerically enriched cyclobutylamines to enantiomerically enriched cyclobutylamides. Such compounds are useful intermediates in the synthesis of microbiocidal thiazole compounds.
专利号:US-2016073631-A1 优先权日:2013-03-04 标 题 :Process for the preparation of dihydropyrrole derivatives 发明人:EL QACEMI MYRIEM; SMITS HELMARS; CASSAYRE JEROME YVES; MULHOLLAND NICHOLAS PHILLIP; RENOLD PETER; GODINEAU EDOUARD; PITTERNA THOMAS 权利人:SYNGENTA PARTICIPATIONS AG; SYNGENTA LTD 摘要:The present invention provides stereoselective processes for the preparation of compounds of formula (I) n n n n n n n n n n n n wherein n P is phenyl, naphthyl, a 6-membered heteroaryl group containing one or two nitrogen atoms as ring members, or a 10-membered bicyclic heteroaryl group containing one or two nitrogen atoms as ring members, and wherein the phenyl, naphthyl and heteroaryl groups are optionally substituted; n R 1 is chlorodifluoromethyl or trifluoromethyl; n R 2 is optionally substituted aryl or optionally substituted heteroaryl; n n is 0 or 1; n including the process comprising n (a-i) reacting a compound of formula II n n n n n n n n n n n n n n n n wherein P, R 1 and R 2 are as defined for the compound of formula I; n with nitromethane in the presence a chiral catalyst to give a compound of formula III n n n n n n n n n n n n n n n n wherein P, R 1 and R 2 are as defined for the compound of formula I; and n (a-ii) reductively cyclising the compound of formula III to give the compound of formula I. n n n n n The invention also provides intermediates useful for processes for the synthesis of compounds of formula (I).
专利号:US-8859522-B2 优先权日:2011-04-27 标题:Processes for the preparation of regadenoson and a new crystalline form thereof 发明人:WOOLDRIDGE LUZVIMINDA T; MA CHUN; NADJI SOURENA 权利人:WOOLDRIDGE LUZVIMINDA T; MA CHUN; NADJI SOURENA; RELIABLE BIOPHARMACEUTICAL CORP 摘要:This disclosure relates to an improved process for the preparation of regadenoson, pharmaceutically acceptable salts thereof, and hydrates thereof, and for the preparation of intermediates useful in the synthesis of regadenoson. The disclosure also relates to a new crystalline form of regadenoson. Processes for the preparation of the crystalline form, compositions containing the crystalline form, and methods of use thereof are also described.
1: Cheng X, Dai T, Hu Z, Cui T, Wang W, Han P, Hu M, Hao J, Liu P, Liu X. Cytochrome P450 and Glutathione S-Transferase Confer Metabolic Resistance to SYP-14288 and Multi-Drug Resistance in Rhizoctonia solani. Front Microbiol. 2022 Mar 21;13:806339. doi: 10.3389/fmicb.2022.806339. 2: Malandrakis AA, Kavroulakis N, Chrysikopoulos CV. Zinc nanoparticles: Mode of action and efficacy against boscalid-resistant Alternaria alternata isolates. Sci Total Environ. 2022 Jul 10;829:154638. doi: 10.1016/j.scitotenv.2022.154638. Epub 2022 Mar 18. 78(6):2240-2249. doi: 10.1002/ps.6845. Epub 2022 Mar 14. 11(3):416. doi: 10.3390/foods11030416. 7: Saifullah S, Margus A, Kankare M, Lindström L. Repeated exposure of fluazinam fungicides affects gene expression profiles yet carries no costs on a nontarget pest. Insect Sci. 2022 Feb 10. doi: 10.1111/1744-7917.13013. Epub ahead of print. 255(3):61. doi: 10.1007/s00425-022-03838-x.
合成参考文献
摘要: 摘要: 摘要:Franke C et al; Chemosphere 29: 1501-14 (1994) 摘要:S109 | PARCEDC | List of 7074 potential endocrine disrupting compounds (EDCs) by PARC T4.2 | DOI:10.5281/zenodo.10944198 参考文献:10.1080/03601234.2019.1634971 摘要:Wang Q, Shen M, Li W, Li W, Zhang F. Controlled-release of fluazinam from biodegradable PLGA-based microspheres. Journal of Environmental Science and Health, Part B. 2019 Jul 02;54(10):810–6. doi: 10.1080/03601234.2019.1634971.