N-甲基羟胺置于盐酸体系中,用 水 作为反应溶剂,以333.4 G的收率获得产物n-甲基羟胺盐酸盐 参考文献: Process To Produce N-Methylydroxylamine Hydrochloride[fr] Procédé De Production De Chloridrate De N-Méthylydroxylamine 标题: Process To Produce N-Methylydroxylamine Hydrochloride[fr] Procédé De Production De Chloridrate De N-Méthylydroxylamine 摘要:该披露提供了改进的制备n-甲基羟胺和n-甲基羟胺盐酸盐的过程.
专利信息
专利号:US-4898952-A 优先权日:1987-05-29 标 题 :Regioselective synthesis of a 1,5-disubstituted pyrazole 发明人:MURRAY WILLIAM V; WACHTER MICHAEL P 权利人:ORTHO PHARMA CORP 摘要:A highly regioselective synthesis of pyrazoles from a mono-substituted hydrazine and a beta -dicarbonyl compound wherein a carboxylic acid moiety is present on the substituent attached to one of the carbonyls. For example, compounds of the formula (I) are formed in marked preference to isomers of formula (IV): (I) (IV)
专利号:US-5714127-A 优先权日:1992-10-08 标题 :System for multiple simultaneous synthesis 发明人:DEWITT SHEILA H H; KIELY JOHN S; PAVIA MICHAEL R; SCHROEDER MEL C; STANKOVIC CHARLES J 权利人:WARNER LAMBERT CO 摘要:A system for the multiple, simultaneous synthesis of compounds preferably uses a reaction apparatus comprising a reservoir rack having a plurality of reaction wells, a plurality of reaction tubes, usually gas dispersion tubes, having filters on their lower ends, a holder block, having a plurality of apertures, and a manifold, which has ports to allow introduction/maintenance of a controlled environment. The manifold top wall has a plurality of apertures in axial alignment with the reaction tubes and a gasket which allows penetration by a needle in order to dispense and aspirate materials from the reaction tubes. Sealing members, such as gaskets, are placed between the holder block, manifold and reservoir rack and the components are releasably fastened together. A robotic sample processor is used to automate the synthesis process using the reaction apparatus.
专利号:US-8951728-B2 优先权日:2004-11-22 标 题:Template directed split and mix synthesis of small molecule libraries 发明人:RASMUSSEN PETER BIRK 权利人:CHEMGENE HOLDING APS 摘要:The invention combines the advantages of split and mix synthesis with the advantages of template directed synthesis. The method comprises the steps of: a) adding a linker molecule L to one or more reaction wells; b) adding a molecule fragment to each of said reaction wells; c) adding an oligonucleotide identifier to each of said reaction wells; d) subjecting said wells to conditions sufficient to allow said molecule fragments and said oligonucleotide identifiers to become attached to said linker molecule, or conditions sufficient for said molecule fragments to bind to other molecule fragments and sufficient for said oligonucleotide identifiers to bind to other oligonucleotide identifiers; e) combining the contents of said one or more reaction wells; and f) contacting the resulting bifunctional molecule(s) of step e) with one or more (oligonucleotide) templates each capable of hybridizing to at least one of the oligonucleotide identifiers added in step c).
专利号:US-5702672-A 优先权日:1992-10-08 标 题 :Apparatus and method for multiple simultaneous synthesis 发明人:DEWITT SHEILA H H; KELL MICHAEL; PAVIA MICHAEL R; KIELY JOHN S; SCHROEDER MEL C; STANKOVIC CHARLES J; WARE STEVEN 权利人:WARNER LAMBERT CO 摘要:An apparatus for multiple, simultaneous synthesis of compounds which consists of: a reservoir block having a plurality of wells; a plurality of reaction tubes, usually gas dispersion tubes, having filters on their lower ends; a holder block, having a plurality of apertures; and a manifold, which may have ports to allow introduction/maintenance of a controlled environment. The manifold top wall has apertures and a detachable plate with identical apertures. The apparatus is constructed from materials which will accommodate heating, cooling, agitation, or corrosive reagents. Gaskets are placed between the components. Rods or clamps are provided for fastening the components together. Apparatus operation involves placing the filters on the lower ends of the reaction tubes in the reservoir block wells, and the upper ends passing through the holder block apertures and into the manifold.
专利号:US-5766556-A 优先权日:1992-10-08 标题:Apparatus and method for multiple simultaneous synthesis 发明人:DEWITT SHEILA HELEN HOBBS; KIELY JOHN STEVEN; PAVIA MICHAEL RAYMOND; SCHROEDER MEL CONRAD; STANKOVIC CHARLES JOHN 权利人:WARNER LAMBERT CO 摘要:An apparatus and method which provides a suitable location for multiple, simultaneous synthesis of compounds. The apparatus consists of: a reservoir block having a plurality of wells; a plurality of reaction tubes, usually gas dispersion tubes, having filters on their lower ends; a holder block, having a plurality of apertures; and a manifold, which may have ports to allow introduction/maintenance of a controlled environment. The manifold top wall has apertures and a detachable plate with identical apertures. The apparatus is constructed from materials which will accommodate heating, cooling, agitation, or corrosive reagents. Gaskets are placed between the components. Rods or clamps are provided for fastening the components together. Apparatus operation involves placing the filters on the lower ends of the reaction tubes in the reservoir block wells, and the upper ends passing through the holder block apertures and into the manifold. The apparatus provides in excess of 1 mg of each product with structural knowledge and control over each compound. The apparatus can be adapted to manual, semiautomatic or fully automatic performance. Using the apparatus a series of building blocks are covalently attached to a solid support. These building blocks are then modified by covalently adding additional different building blocks or chemically modifying some existing functionality until the penultimate structure is achieved. This is then cleaved from the solid support by another chemical reaction into the solution within the well yielding an array of newly synthesized individual compounds, which after postreaction modification, if necessary, are suitable for testing for activity.
专利号:US-5567391-A 优先权日:1992-10-08 标题 :Apparatus for multiple simultaneous synthesis 发明人:DEWITT SHEILA H H; KIELY JOHN S; PAVIA MICHAEL R; SCHROEDER MEL C; STANKOVIC CHARLES J 权利人:WARNER LAMBERT CO 摘要:An apparatus and method which provides a suitable location for multiple, simultaneous synthesis of compounds. The apparatus consists of: a reservoir block having a plurality of wells; a plurality of reaction tubes, usually gas dispersion tubes, having filters on their lower ends; a holder block, having a plurality of apertures; and a manifold, which may have ports to allow introduction/maintenance of a controlled environment. The manifold top wall has apertures and a detachable plate with identical apertures. The apparatus is constructed from materials which will accommodate heating, cooling, agitation, or corrosive reagents. Gaskets are placed between the components. Rods or clamps are provided for fastening the components together. Apparatus operation involves placing the filters on the lower ends of the reaction tubes in the reservoir block wells, and the upper ends passing through the holder block apertures and into the manifold. The apparatus provides in excess of 1 mg of each product with structural knowledge and control over each compound. The apparatus can be adapted to manual, semiautomatic or fully automatic performance. Using the apparatus a series of building blocks are covalently attached to a solid support. These building blocks are then modified by covalently adding additional different building blocks or chemically modifying some existing functionality until the penultimate structure is achieved. This is then cleaved from the solid support by another chemical reaction into the solution within the well yielding an array of newly synthesized individual compounds, which after postreaction modification, if necessary, are suitable for testing for activity.
[参考文献]: A A Spooren, Et Al. In Vitro Haematotoxic Effects Of Three Methylated Hydroxylamines. Arch Toxicol. 1997;71(5):299-305. [参考文献]: C T Evelo, Et Al. Two Mechanisms For Toxic Effects Of Hydroxylamines In Human Erythrocytes: Involvement Of Free Radicals And Risk Of Potentiation. Blood Cells Mol Dis. 1998 Sep;24(3):280-95. [参考文献]: J C Swarts, Et Al. Kinetic Studies On The Reduction Of The Tyrosyl Radical Of The R2 Subunit Of E. Coli Ribonucleotide Reductase. Biochim Biophys Acta. 1995 Mar 15;1247(2):215-24. [参考文献]: J Taira, Et Al. Nitric Oxide Formation From Hydroxylamine By Myoglobin And Hydrogen Peroxide. Biochim Biophys Acta. 1997 Oct 20;1336(3):502-8. [参考文献]: K Stolze, Et Al. Free Radical Intermediates In The Oxidation Of N-Methylhydroxylamine And N,N-Dimethylhydroxylamine By Oxyhemoglobin. Free Radic Res Commun. 1990;8(2):123-31.
合成参考文献
摘要:Merino, P., Science of Synthesis Knowledge Updates, (2010) 4, 340.