在 氨体系中,用 乙醚,甲苯 作为反应溶剂,以75%的收率获得产物三氟乙酸铵 参考文献:Interaction Of Fluoroalkyl-Containing-Diketones With Amines 标题:Interaction Of Fluoroalkyl-Containing-Diketones With Amines 摘要:The Composition Of Products Of The Interaction Of Asymmetric Fluoroalkyl-Containing Beta-Diketones With Amines Was Studied. Mixtures Of Regioisomeric Beta-Aminovinylketones And Products Of Cleavage And Secondary Condensation Are Formed,Depending On The Temperature,The Solvent,The Nature Of The Fluorinated And Nonfluorinated Substituents In The Beta-Diketone,And The Basicity Of The Amine. The Major Product Is A Beta-Aminovinylketone In Which The Nh2 Group Is Removed From The Fluoroalkyl Substituent. No Beta-Aminovinylimines,Products Of Condensation Involving Two Electrophilic Centers,Were Observed. DOI:10.1007/bf01430731
专利号:US-6683189-B1 优先权日:1996-02-26 标 题 :Method for the synthesis of pyrrole and imidazole carboxamides on a solid support 发明人:DERVAN PETER B; BAIRD ELDON 权利人:CALIFORNIA INST OF TECHN 摘要:The present invention describes a novel method for the solid phase synthesis of polyamides containing imidazole and pyrrole carboxamides. The polyamides are prepared on a solid support from aromatic carboxylic acids and aromatic amines with high stepwise coupling yields (>99%), providing milligram quantities of highly pure polyamides. The present invention also describes the synthesis of analogs of the natural products Netropsin and Distamycin A, two antiviral antibiotics. The present invention also describes a novel method for the solid phase synthesis of imidazole and pyrrole carboxamide polyamide-oligonucleotide conjugates. This methodology will greatly increase both the complexity and quantity of minor-groove binding polyamides and minor-groove binding polyamide-oligonucleotide conjugates which can be synthesized and tested.
专利号:WO-03031376-A1 优先权日:2001-10-12 标 题 :Solid phase synthesis of substituted 1,5-benzodiazepine-2-one and 1,5-benzothiazepine-2-one 发明人:MORTON GEORGE C; SALVINO JOSEPH M; LABAUDINIERE RICHARD F; HERPIN TIMOTHY F 权利人:AVENTIS PHARMA INC; MORTON GEORGE C; SALVINO JOSEPH M; LABAUDINIERE RICHARD F; HERPIN TIMOTHY F 摘要:A solid phase synthetic method for making substituted 1,5-benzodiazepine-2-one or 1,5-benzothiazepine-2-one. The method is useful for synthesis of large numbers of compounds through automated parallel synthesis or combinatorial library generation and is thus important to rapid discovery or new therapeutic agents containing the base structure of 1,5-benzodiazepine-2-one or 1,5-benzothiazepine-2-one.
专利号:US-2009093630-A1 优先权日:2007-09-21 标题:Chiral synthesis of diazepinoquinolines 发明人:MEGATI SREENIVASULU; BHANSALI SHILPA; DEHNHARDT CHRISTOPH; DESHMUKH SUBODH; FUNG PETER; MACEWAN MICHAEL; TINDER ROBERT J 权利人:WYETH CORP 摘要:The present invention relates to improved methods of resolution and recrystallization for synthesizing compounds useful as 5HT 2C agonists or partial agonists, including intermediates thereto.
专利号:EP-1404682-B1 优先权日:2001-06-29 标题:Method of inhibiting ptp 1b and/or t-cell ptp and/or other ptpases with an asp residue at position 48 发明人:HANSEN THOMAS KRUSE; OLSEN OLE HVILSTED; PETERSEN ANDERS KLARSKOV; LAU JESPER; ANDERSEN HENRIK SUNE; MOLLER NIELS PETER HUNDAHL 权利人:NOVO NORDISK AS 摘要:This invention relates to oxalylamide inhibitors of Protein Tyrosine Phosphatase 1B (PTP1B) and/or T-cell Protein Tyrosine Phosphatase (TC-PTP) and/or Protein Tyrosine Phosphatases (PTPases) having an aspartic acid (Asp) in position 48 (PTP1B numbering, Chernoff et al., Proc. Natl. Acad. Sci. USA 87: 2735-2789 (1989)) and a method of inhibiting such PTPases by exposing the enzyme to inhibitor compounds of formula 1. This invention also relates to (I) the design and selection of inhibitors, which bind to the active site of PTP1B and/or TC-PTP and/or PTPases having an aspartic acid (Asp) in position 48 (II) the synthesis of said inhibitors, methods for their preparation and (III) to compositions comprising the inhibitor compounds.
专利号:US-3992436-A 优先权日:1976-01-02 标题:Synthesis of oxalate esters from carbon monoxide and carboxylic ortho esters 发明人:ZEHNER LEE R 权利人:ATLANTIC RICHFIELD CO 摘要:A process for the preparation of oxalate esters by the catalytic oxidative carbonylation of carboxylic ortho esters with carbon monoxide and oxygen-containing gas in the presence of a metal salt catalyst, an amine base and a catalytic amount of an alcohol. Preferably a catalytic amount of particular metal oxidizing salts is employed along with a catalytic amount of an acid or an amine salt compound. Alternatively various counterions and ligands of the metal salt catalysts may be employed.
专利号:US-4005131-A 优先权日:1976-01-02 标 题 :Synthesis of oxalate esters from carbon monoxide and acetals or ketals 发明人:ZEHNER LEE R 权利人:ATLANTIC RICHFIELD CO 摘要:A process for the preparation of oxalate esters by the catalytic oxidative carbonylation of acetals and ketals with carbon monoxide and oxygen-containing gas in the presence of a metal salt catalyst, an amine base and a catalytic amount of an alcohol. Preferably a catalytic amount of particular metal oxidizing salts is employed along with a catalytic amount of an acid or an amine salt compound. Alternatively various counterions and ligands of the metal salt catalysts may be employed.
[参考文献]: V Scott Sharp, Et Al. Stereoselective High-Performance Liquid Chromatography And Analytical Method Characterization Of Evacetrapib Using A Brush-Type Chiral Stationary Phase: A Challenging Isomeric Separation Requiring A Unique Eluent System. J Chromatogr A. 2014 Oct 10:1363:183-90.
合成参考文献
参考文献:10.1038/s42003-020-01518-8 摘要:Dumitru AC, Deepak RNVK, Liu H, Koehler M, Zhang C, Fan H, Alsteens D. Submolecular probing of the complement C5a receptor–ligand binding reveals a cooperative two-site binding mechanism. Communications Biology. 2020 Dec 18;3(1):786. doi: 10.1038/s42003-020-01518-8. 参考文献:10.1007/s11237-022-09713-w 摘要:Kozytskiy AV, Bielousov OP. Photocatalytic C(sp3)–H Activation of Aliphatic Amines by Using Decatungstate Anion to Obtain Aminoacids. Theoretical and Experimental Chemistry. 2022 Jan;57(6):437–42. doi: 10.1007/s11237-022-09713-w.