甲基硝基苯置于sodium Hydroxide,双氧水,Sodium Ethanolate体系中,化学反应生成2-硝基苯乙酸 参考文献:Di Carlo,Journal Of The American Chemical Society,1944,Vol. 66,P. 1420 标题:Di Carlo,Journal Of The American Chemical Society,1944,Vol. 66,P. 1420
专利号:US-7109377-B2 优先权日:1996-10-16 标 题:Synthesis of combinatorial libraries of compounds reminiscent of natural products 发明人:SCHREIBER STUART L; SHAIR MATTHEW D; TAN DEREK S; FOLEY MICHAEL A; STOCKWELL BRENT R 权利人:HARVARD COLLEGE 摘要:The present invention provides complex compounds reminiscent of natural products and libraries thereof, as well as methods for their production. The inventive compounds and libraries of compounds are reminiscent of natural products in that they contain one or more stereocenters, and a high density and diversity of functionality. In general, the inventive libraries are synthesized from diversifiable scaffold structures, which are synthesized from readily available or easily synthesizable template structures. In certain embodiments, the inventive compounds and libraries are generated from diversifiable scaffolds synthesized from a shikimic acid based epoxyol template. In other embodiments, the inventive compounds and libraries are generated from diversifiable scaffolds synthesized from the pyridine-based template isonicotinamide. The present invention also provides a novel ortho-nitrobenzyl photolinker and a method for its synthesis. Furthermore, the present invention provides methods and kits for determining one or more biological activities of members of the inventive libraries. Additionally, the present invention provides pharmaceutical compositions containing one or more library members.
专利号:US-3978140-A 优先权日:1974-09-23 标题 :Process for the preparation of carbinols 发明人:LANE CLINTON FISHER; MYATT HAL LESLIE 权利人:ALDRICH BORANES INC 摘要:Organic compounds containing a carboxylic acid or carboxylic acid anhydride group are reduced when contacted with an alkali metal borohydride and a boron trihalide in a liquid medium in which diborane is soluble in the form of a labile borane adduct. Hydrolysis of the reaction mixture then provides a useful synthesis of the corresponding carbinols. n The alkali metal borohydride-boron trihalide reagent may either be preformed and reacted subsequently with an organic compound containing a carboxylic acid or anhydride group, or the alkali metal borohydride-boron trihalide reagent may be produced in the presence of an organic compound containing a carboxylic acid or anhydride group. This development makes it possible to synthesize a wide variety of carbinols which are valuable and useful intermediates in organic synthesis.
专利号:US-5446186-A 优先权日:1993-11-09 标 题:Structure and synthesis of nitrophenyl-EGTA, a caged calcium, intermediates thereof and a method of producing a high photochemical yield of liberated calcium 发明人:ELLIS-DAVIES GRAHAM C R; KAPLAN JACK H 摘要:The synthesis and compound of a new caged calcium which is an ortho-nitrophenyl derivative of EGTA and various intermediates. It is synthesized in ten steps and 24% overall yield. The photosensitive chelator, nitrophenyl-EGTA, has a K d for Ca 2+ of 80 nM and for Mg 2+ of 8.8 mM. Upon exposure to ultra-violet light (in the region of 350 nm), the chelator is cleaved, yielding iminodiacetic acid photoproducts with known low Ca-affinity (K d =1 mM). The quantum yield of photolysis of nitrophenyl-EGTA in the presence of Ca a+ is 0.23 and in the absence of Ca 2+ is 0.20. In experiments with chemically skinned skeletal muscle fibers, a fully relaxed fiber equilibrated with nitrophenyl-EGTA:Ca 2+ complex, in the presence of physiological [Mg 2+ ] (i.e. 1.0 mM), produced maximal contraction after a single flash from a frequency doubled ruby laser (347 nm). Half-maximal tension was achieved in 18 ms at 15° C. Nitrophenyl-EGTA provides a new tool for the investigation of the mechanism of Ca 2+ -dependent physiological processes, since under conditions of normal intracellular Ca 2+ and Mg 2+ ions, only Ca 2+ ions are bound by the photolabile chelator and on illumination are released rapidly and in high photochemical yield.
专利号:US-9346892-B2 优先权日:2011-03-18 标题 :Methods for synthesis of an oligopeptide microarray 发明人:ALBERT TOM; RICHMOND TODD; RODESCH MATTHEW; STENGELE KLAUS-PETER; BUEHLER JOCHEN; OTT MARKUS 权利人:ALBERT TOM; RICHMOND TODD; RODESCH MATTHEW; STENGELE KLAUS-PETER; BUEHLER JOCHEN; OTT MARKUS; ROCHE NIMBLE GEN INC 摘要:An oligopeptide microarray and methods for the synthesis thereof are presented. Further presented is a microarray on a solid support comprising at least about 10,000 oligopeptide features per cm 2 and preferably at least about 50,000 oligopeptide features per cm 2 .
专利号:WO-2015071493-A1 优先权日:2013-11-18 标题:Chemoenzymatic synthesis of the cephalosporine intermediate 7-amino-3-alkenylcephem-4-carboxylic acid 发明人:ZEPECK FERDINAND; SCHLEICH HERBERT; TOTSCHNIG KLAUS; KAMMEL WOLFGANG; REMLER PETER; SEISSER BIRGIT; STROHMEIER GERNOT 权利人:SANDOZ AG 摘要:The invention relates to processes for the preparation of 7-amino-3- alkenylcephem-4-carboxylic acid of Formula 6 and the compounds of Formula 2 and 5 by using the enzymes p-nitrobenzyl esterase and penicillin G amidase. The processes either start from the compound of Formula 1 or the compound of Formula 5.
专利号:US-10662145-B2 优先权日:2018-08-17 标题:Method of synthesizing diclofenac sodium 发明人:CHEN FENER; WANG LINGDONG; MENG GE; HUANG ZEDU; CHENG DANG; PENG HAIHUI; LIANG GUANFENG 权利人:UNIV FUDAN 摘要:The invention relates to the chemical synthesis of pharmaceutical API, and specifically to a method of synthesizing diclofenac sodium, which is a kind of nonsteroidal anti-inflammatory drug for relieving pain. The method includes: nitrating phenylacetate to prepare o-nitrophenylacetate (2); hydrogenating o-nitrophenylacetate (2) to prepare o-aminophenylacetate (3); amidating an amino group of o-aminophenylacetate (3) to obtain 2-(2-benzoylaminophenyl) acetate (4); 2-(2-benzoylaminophenyl) acetate (4) reacting with thionyl chloride to prepare a chloroimine intermediate, and then condensing the intermediate of chloroimine with 2,6-dichlorophenol using an inorganic base to prepare (E)-methyl-2-(2-((2,6-dichlorophenoxy)(phenyl)methyleneamino) phenyl ester (5); subjecting (E)-methyl-2-(2-((2,6-dichlorophenoxy)(phenyl)methyleneamino) phenyl ester (5) to Chapman rearrangement to afford methyl 2-(2-(N-(2,6-dichlorophenyl)benzoylamino)phenyl) ester (6); and hydrolyzing methyl 2-(2-(N-(2,6-dichlorophenyl)benzoylamino)phenyl) ester (6) to provide the target compound as of diclofenac sodium API. The overall yield is up to 67% based on methyl phenylacetate.
[参考文献]: Eric Franqueville, Et Al. Studies On The Catalytic Behaviour Of A Cholinesterase-Like Abzyme In An Aot Microemulsion System. J Biotechnol. 2002 Aug 7;97(2):177-82. [参考文献]: H U Schulz, Et Al. Determination Of The Theophylline Solubilizer Salicylamide-O-Acetic Acid In Serum And Urine Using High-Performance Liquid Chromatography. J Pharm Biomed Anal. 1985;3(5):469-75. [参考文献]: Jan-Michael Mewes, Et Al. Molecular Mechanism Of Uncaging Co2 From Nitrophenylacetate Provides General Guidelines For Improved Ortho-Nitrobenzyl Cages. Chemphyschem. 2011 Aug 1;12(11):2077-80. [参考文献]: M K Danks, Et Al. Comparison Of Activation Of Cpt-11 By Rabbit And Human Carboxylesterases For Use In Enzyme/prodrug Therapy. Clin Cancer Res. 1999 Apr;5(4):917-24. [参考文献]: Manuela F Frasco, Et Al. Mechanisms Of Cholinesterase Inhibition By Inorganic Mercury. Febs J. 2007 Apr;274(7):1849-61.
合成参考文献
摘要:Joule, J. A., Science of Synthesis Knowledge Updates, (2010) 2, 401. 摘要:Riva, R.; Banfi, L.; Basso, A., Science of Synthesis: Multicomponent Reactions, (2013) 1, 381. 摘要:Zhang, M.; Su, W., Science of Synthesis: Catalytic Transformations via CH Activation, (2015) 1, 96. 摘要:Fukuta, T.; Kanai, M., Science of Synthesis: Cross-Dehydrogenative Coupling, (2023) nan, 439.