2-碘苯甲酸乙酯,置于copper(I) Oxide,Bis(1,5-Cyclooctadiene)Nickel (0),Caesium Carbonate,1,3-二均三甲苯基咪唑-2-叉体系中,用 N,N-二甲基甲酰胺,甲苯 用作溶剂,化学反应 32.0H,反应生成1-苯基吡唑 参考文献:Nickel-Catalyzed Reductive Defunctionalization Of Esters In The Absence Of An External Reductant: Activation Of C-o Bonds 标题:Nickel-Catalyzed Reductive Defunctionalization Of Esters In The Absence Of An External Reductant: Activation Of C-o Bonds 摘要:镍催化剂在无外部还原剂的情况下,报告了酯的还原裂解,其中涉及对惰性酰基c-O键进行裂解,这种裂解发生在o-烷基酯中. Doi:10.1039/c9Cc07710C
专利号:US-12221421-B2 优先权日:2019-03-19 标题:Process for synthesis of Fipronil 发明人:GHARDA KEKI HORMUSJI; SHENOY DIWAKAR; SHET LAXMINARAYAN; SAMANGADKAR YATIN; KAWADE ABHIJEET SURESH 权利人:GHARDA CHEMICALS LTD 摘要:A process for the synthesis of fipronil, which is a broad spectrum insecticide of the following chemical structure, is provided.The process provides fipronil with a yield in the range of 75% to 90% and purity in the range of 95% to 97%. By the process, the observed amount of sulfone impurity i.e., 5-amino-1-(2,6-dichloro-4-trifluoromethylphenyl)-3-cyano-4-trifluoro methylsulfonyl pyrazole in fipronil is in the range of 0% to 0.5%.
专利号:WO-2010049789-A1 优先权日:2008-10-27 标 题 :Process for the synthesis of fipronil 发明人:JUELICH ALEXANDER; TILLICH JOACHIM 权利人:DYNAMIT NOBEL AG; JUELICH ALEXANDER; TILLICH JOACHIM 摘要:This invention relates to a process for the continuous synthesis of 5-amino-1-[2,6- dichloro-4-(rifluoromethyl)phenyl]-4-(rifluoromethylsulfinyl)-1H-pyrazole-3-carbonitrile comprising the step of reacting in a solvent 5-amino-1-[2,6-dichloro-4- (trifluoromethyl)phenyl]-4-(trifluoromethylthio)-1H-pyrazole-3-carbonitrile with an oxidizing agent. The process provides a more efficient and more robust process than the existing processes.
专利号:US-6271375-B1 优先权日:1997-06-30 标 题 :Ortho-metalation process for the synthesis of 2-substituted-1-(tetrazol-5-yl)benzenes 发明人:VILLA MARCO; ALLEGRINI PIETRO; ARRIGHI KATIUSCIA; PAIOCCHI MAURIZIO 权利人:ZAMBON SPA 摘要:A process of direct metalation of phenyltetrazoles useful for preparing compounds of formula (II) intermediates for the synthesis of angiotensin II antagonists is described.
专利号:US-9453044-B2 优先权日:2012-02-07 标题 :Method of synthesizing peptides, proteins and bioconjugates 发明人:LIU CHUAN FA; ZHAO JUNFENG 权利人:UNIV NANYANG TECH 摘要:The invention relates to the synthesis of peptides, proteins and related bioconjugates, and in particular, to such synthesis using a peptide ligation method whereby a C-terminal salicylaldehyde ester peptide is reacted with an aminoacyl-N-hydroxl peptide. The invention also relates to the synthesis of cyclic peptides, including serinyl- or threonyl-containing cyclic peptides. The invention further relates to a solid phase synthesis of C-terminal salicylaldehyde ester peptides.
专利号:US-7781488-B2 优先权日:2002-06-10 标 题:Post-cleavage sulfur deprotection for convergent protein synthesis by chemical ligation 发明人:BOTTI PAOLO; VILLAIN MATTEO; MANGANIELLO SONIA; GAERTNER HUBERT 权利人:AMYLIN PHARMACEUTICALS INC 摘要:The present invention provides a method and compositions for synthesizing an oligopeptide or polypeptide by convergent assembly of a plurality of pairs of oligopeptides in chemical ligation reactions. An important aspect of the present invention is an oligopeptide having a C-terminal disulfide-protected carboxythioester group that can be deprotected to spontaneously generate a free C-terminal thioester moiety. This allows a single precursor to participate in a succession of chemical ligation reactions, thereby making the convergent synthesis approach possible. The present invention is useful in methods for chemical synthesis of oligopeptides, polypeptides and proteins, and improves the efficiency of native chemical ligation reactions, particularly where four or more peptide fragments are used to assemble an oligopeptide, polypeptide or protein product.
专利号:US-6747175-B2 优先权日:2000-03-01 标 题:Chlorination of an aniline in a hydrofluoric medium 发明人:KEMPF HUBERT; GUIDOT GILBERT; SAINT-JALMES LAURENT 权利人:RHODIA CHIMIE SA 摘要:The invention concerns a method for the synthesis of chlorinated aniline on the ring and comprising at least a sp3 hybridization carbon atom both perhalogenated and bearing a fluorine atom. Said method is characterized in that it comprises a step which consists in chlorinating a precursor aniline of said chlorinated aniline, said chlorination being carried out in a hydrofluoric medium capable of exchanging chlorine and fluorine in benzyl position. The invention is useful for the synthesis of organofluorinated and/or chlorinated compounds.
[参考文献]: Indira Fabre, Et Al. Autocatalytic Intermolecular Versus Intramolecular Deprotonation In C-H Bond Activation Of Functionalized Arenes By Ruthenium(Ii) Or Palladium(Ii) Complexes. Chemistry. 2013 Jun 3;19(23):7595-604. [参考文献]: Nobuyoshi Umeda, Et Al. Rhodium-Catalyzed Oxidative 1:1, 1:2, And 1:4 Coupling Reactions Of Phenylazoles With Internal Alkynes Through The Regioselective Cleavages Of Multiple C-H Bonds. J Org Chem. 2011 Jan 7;76(1):13-24.
合成参考文献
摘要:Götzinger, A. C.; Müller, T. J. J., Science of Synthesis Knowledge Updates, (2017) 3, 214. 摘要:Götzinger, A. C.; Müller, T. J. J., Science of Synthesis Knowledge Updates, (2017) 3, 181. 摘要:Rudzinski, D. M.; Leadbeater, N. E., Science of Synthesis Knowledge Updates, (2012) 1, 406. 摘要:Ahmad, O. K.; Movassaghi, M., Science of Synthesis: Cross Coupling and Heck-Type Reactions, (2012) 2, 211. 摘要:Ahmad, O. K.; Movassaghi, M., Science of Synthesis: Cross Coupling and Heck-Type Reactions, (2012) 2, 212.