专利号:US-6800785-B1 优先权日:2002-10-15 标题:Process for the synthesis of estrogen receptor modulators 发明人:MENG DONGFANG 权利人:MERCK & CO INC 摘要:The present invention relates to processes for the synthesis of intermediates useful for the synthesis of estrogen receptor modulators. The process includes new methods for annelating 5-, 6- and 7-membered cycloalkenones onto an indanone.
专利号:US-6423871-B1 优先权日:1999-02-26 标题 :Efficient synthesis of secondary amines by selective alkylation of primary amines 发明人:JUNG KYUNG WOON 权利人:UNIV SOUTH FLORIDA 摘要:A method for selective mono-N-alkylation of primary amines to produce secondary amines that are substantially free of overalkylated tertiary amines and quaternary ammonium salts, under mild reaction conditions without the necessity of protecting groups. Compounds of the class of secondary amines are produced by reacting an alkyl halide with an alkyl amine in anhydrous solvent, preferably dimethyl sulfoxide or N,N-dimethylformamide, in the presence of 0.1 to 3 molar equivalents of a cesium base. Optionally, the extent and selectivity of mono-N-alkylation is enhanced by addition to the reaction mixture of a powdered molecular sieve material for removal of water produced by the reaction, and/or tetrabutylammonium iodide to promote halide exchange. The invention permits selective and efficient mono-N-alkylation of a wide variety of substrates at 23° C.; does not cause racemization when used with enantiomerically-pure chiral substrates such as L-α-aminoesters; and is applied to solid phase synthesis whereby either the alkyl amine or alkyl halide is immobilized. The method is additionally used to produce polyamines, such as N-(2-(2-aminoethylthio)ethyl)ethylenediamine in 73% yield.
专利号:WO-0050377-A1 优先权日:1999-02-26 标 题:Efficient synthesis of secondary amines by selective alkylation of primary amines 发明人:JUNG KYUNG WOON 权利人:UNIV SOUTH FLORIDA 摘要:A method for selective mono-N-alkylation of primary amines to produce secondary amines that are substantially free of overalkylated tertiary amines and quaternary ammonium salts, under mild reaction conditions without the necessity of protecting groups. Compounds of the class of secondary amines are produced by reacting an alkyl halide with an alkyl amine in anhydrous solvent, preferably dimethyl sulfoxide or N,N-dimethylformamide, in the presence of 0.1 to 3 molar equivalents of a cesium base. Optionally, the extent and selectivity of mono-N-alkylation is enhanced by addition to the reaction mixture of a powdered molecular sieve material for removal of water produced by the reaction, and/or tetrabutylammonium iodide to promote halide exchange. The invention permits selective and efficient mono-N-alkylation of a wide variety of substrates at 23 °C; does not cause racemization when used with enantiomerically-pure chiral substrates such as L-α-aminoesters; and is applied to solid phase synthesis whereby either the alkyl amine or alkyl halide is immobilized. The method is additionally used to produce polyamines, such as N-(2-(2-aminoethylthio)ethyl)ethylenediamine in 73 % yield.
专利号:US-9988492-B2 优先权日:2013-09-30 标题:Methods for post-fabrication functionalization of poly(ester ureas) 发明人:BECKER MATTHEW; LIN FEI 权利人:BECKER MATTHEW; LIN FEI; UNIV AKRON 摘要:Amino acid-based poly(ester urea)s (PEU) are emerging as a class of polymers that have shown promise in regenerative medicine applications. Embodiments of the invention relate to the synthesis of PEUs carrying pendent “clickableâ€? groups on modified tyrosine amino acids. The pendent species include alkyne, azide, alkene, tyrosine-phenol, and ketone groups. PEUs with M w exceeding 100k Da were obtained via interfacial polycondensation methods and the concentration of pendent groups was varied by copolymerization. The incorporation of derivatizable functionalities is demonstrated using 1 H NMR and UV-Vis spectroscopy methods. Electrospinning was used to fabricate PEU nanofibers with a diameters ranging from 350 nm to 500 nm. The nanofiber matricies possess mechanical strengths suitable for tissue engineering (Young's modulus: 300±45 MPa; tensile stress: 8.5±1.2 MPa). A series of bioactive peptides and fluorescent molecules were conjugated to the surface of the nanofibers following electrospinning using bio-orthogonal reactions in aquous media.
专利号:US-2007015793-A1 优先权日:2003-12-23 标 题:Synthesis of nojirimycins 发明人:HIRTH BRADFORD H; RENNIE GLEN 权利人:MACROZYME DNM B V 摘要:Disclosed are methods of preparing substituted nojirimycins represented by the following formula, n n ncomprising reacting 1-deoxynojirimycin with a reagent prepared by reacting an oxidizing agent with the compound represented by the following formula.
专利号:US-8674143-B2 优先权日:2008-10-15 标 题 :Synthesis of green ketone intermediate 发明人:BONRATH WERNER; LETINOIS ULLA; SCHUETZ JAN 权利人:BONRATH WERNER; LETINOIS ULLA; SCHUETZ JAN; DSM IP ASSETS BV 摘要:A process for the preparation of 1-ethynyl-3,3-dimethylcyclohexan-1-ol from dimedone by a reaction sequence of reduction and ethynylation and its further transformation into green ketone.
参考标题:Total Synthesis Of (−)-Sarain A 作者:Michael H. Becker,Peter Chua,Robert Downham,Christopher J. Douglas,Neil K. Garg,Sheldon Hiebert,Stefan Jaroch,Richard T. Matsuoka,Joy A. Middleton,Fay W. Ng,Larry E. Overman |发布日期:2007.10.1 摘要:Studies Toward The Complex Marine Alkaloid Sarain A. Various Strategies Were Conceived, Setbacks Encountered, And Solutions Developed, Ultimately Leading To A Successful Enantioselective Total Synthesis. Our Route To (+)-Sarain A Features A Number Of Key Steps, Including An Asymmetric Michael Addition To Install The C4'-C3'-C7' Stereotriad, An Enoxysilane-N-Sulfonyliminium Ion Cyclization To Set The C3 Quaternary
合成参考文献
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