Solution containing a nitroxide radical for magnetometry by nuclear
magnetic resonance
    2.
    发明授权
    Solution containing a nitroxide radical for magnetometry by nuclear magnetic resonance 失效
    含有核磁共振磁力计的氮氧自由基的溶液

    公开(公告)号:US5681753A

    公开(公告)日:1997-10-28

    申请号:US568757

    申请日:1995-12-07

    摘要: The invention relates to a solution containing a nitroxide radical for magnetometry by nuclear magnetic resonance. This solution is constituted by a nitroxide radical of formula: ##STR1## in which R.sup.1, R.sup.2, R.sup.3 and R.sup.4, which can be the same or different, represent an alkyl group or an alkoxy group which may be deuterated, or in which the pairs R.sup.1 -R.sup.2 and/or R.sup.3 -R.sup.4 together form an optionally deuterated cycloalkyl or polycycloalkyl group, and N represent .sup.14 N or .sup.15 N, dissolved in a solvent having an oxidizing power and an appropriate viscosity. The solvent can be constituted by a mixture of water and two compounds respectively playing the part of the oxidizing agent and viscosity modifying agent, e.g. water, ethylene glycol and NalO.sub.4, or can be solely constituted by a mixture of water and an oxidizing agent able to modify the viscosity, such as acetic acid.

    摘要翻译: 本发明涉及含有用于通过核磁共振进行磁力计的氮氧自由基的溶液。 该溶液由式(I)的氮氧自由基构成,其中可以相同或不同的R 1,R 2,R 3和R 4表示可以被氘化的烷基或烷氧基,或 其中对R1-R2和/或R3-R4一起形成任选的氘代环烷基或多环烷基,N代表14N或15N,溶解在具有氧化能力和适当粘度的溶剂中。 溶剂可以由水和两种化合物的混合物构成,分别在氧化剂和粘度调节剂的一部分中播放。 水,乙二醇和NalO 4,或者可以由水和能够改变粘度的氧化剂的混合物,例如乙酸构成。

    Free radicals
    4.
    发明授权
    Free radicals 失效
    自由基

    公开(公告)号:US5530140A

    公开(公告)日:1996-06-25

    申请号:US220522

    申请日:1994-03-31

    摘要: The invention provides novel persistent free radicals useful in Overhauser MRI being triarylmethyl radicals having as at least one aryl group a group of formula ##STR1## (wherein each X which may be the same or different is an oxygen or sulphur atom or a group CO or S(O).sub.n, (where n is 1 to 3) with the proviso that at least one group X is a sulphur atom or a S(O).sub.n group; R.sup.1 is a hydrogen atom or group of formula --M, --XM, --X--Ar.sup.2, or --Ar.sup.2 where M is a water solubilizing group, and Ar.sup.2 represents a 5-10 membered aromatic ring optionally substituted by a water solubilizing group M; and each of the groups R.sup.7, which may be the same or different, is a hydrogen atom, or a hydrocarbon group or a water solubilizing group M, or two groups R.sup.7 together with the atom to which they are bound represent a carbonyl group or a 5 to 8 membered cycloalkylidene, mono- or di-oxacycloalkylidene, mono- or di-azacycloalkylidene or mono- or di-thiacycloalkylidene group optionally with the ring attachment carbon replaced by a silicon atom, and R.sup.7 where it is other than hydrogen, is optionally substituted by a hydroxyl group, an optionally alkoxylated, optionally hydroxylated acyloxy or alkyl group or a water solubilizing group M)). The novel radicals have good stability, long relaxation times and good relaxivity.

    摘要翻译: 本发明提供了在Overhauser MRI中有用的新型持久性自由基,其具有作为至少一个芳基的基团为具有下式的基团的三芳基甲基(其中可以相同或不同的X是氧或硫原子或 基团CO或S(O)n,(其中n为1至3),条件是至少一个基团X为硫原子或S(O)n基团; R 1为氢原子或式-M ,-XM,-X-Ar2或-Ar2,其中M是水溶性基团,Ar2表示任选被水增溶基团M取代的5-10元芳香环;并且各基团R7可以是 相同或不同的是氢原子,或烃基或水溶性基团M,或两个R 7与它们所连接的原子一起代表羰基或5-8元环亚烷基,单 - 或二 - 单环或二氮杂环亚烷基或任选具有环连接c的单 - 或二 - 芳烃被硅原子取代,并且其中不是氢的R 7任选被羟基取代,任选烷氧基化,任选羟基化的酰氧基或烷基或水溶性基团M))。 新型自由基具有良好的稳定性,较长的松弛时间和良好的松弛性。

    Selective isotopic labeling of spin labels for electron spin resonance
spectroscopy
    5.
    发明授权
    Selective isotopic labeling of spin labels for electron spin resonance spectroscopy 失效
    电子自旋共振光谱自旋标记的选择性同位素标记

    公开(公告)号:US5431901A

    公开(公告)日:1995-07-11

    申请号:US227793

    申请日:1988-08-03

    摘要: Selective isotopic-labeling of spin label compounds, used in electron spin resonance spectroscopy to detect, measure and monitor the presence of paramagnetic species, increases the sensitivity of the electron spin resonance technique in assays for paramagnetic species, such as the determination of oxygen tension in solution or in a biological sample, like a living organism. Spin label compounds, such as nitroxides, like 3-carbamoyl-2,2,5,5-tetramethyl-3-pyrroline-1-yloxyl (CTPO), are selectively, but not completely, isotopically-labeled, such as partially deuterated, to increase the sensitivity and reliability of assays employing electron spin resonance spectroscopic measurements.

    摘要翻译: 用于电子自旋共振光谱法的自旋标记化合物的选择性同位素标记用于检测,测量和监测顺磁性物质的存在,增加了电子自旋共振技术在顺磁性物质的测定中的灵敏度,例如测定氧气张力 溶液或生物样品,如活体。 旋转标记化合物,例如硝基氧,如3-氨基甲酰基-2,2,5,5-四甲基-3-吡咯啉-1-基氧基(CTPO),是选择性但不完全同位素标记的,例如部分氘代, 以提高使用电子自旋共振光谱测量的测定的灵敏度和可靠性。

    Process for the Oxidation of Secondary Amines into the Corresponding Nitroxides
    6.
    发明申请
    Process for the Oxidation of Secondary Amines into the Corresponding Nitroxides 有权
    将二胺氧化成相应的硝基氧化物的方法

    公开(公告)号:US20100305322A1

    公开(公告)日:2010-12-02

    申请号:US12854677

    申请日:2010-08-11

    IPC分类号: C07D211/44 C07D491/113

    摘要: The invention relates to a process for the preparation of secondary nitroxide radicals from their corresponding secondary amines by oxidation with an organic peracid, comprising the steps a) adding to a reaction vessel a secondary amine, optionally together with an organic solvent and in one batch a base selected from the group consisting of alkali metal, alkaline earth metal or ammonium bicarbonates and alkaline earth metal or ammonium carbonates or mixtures thereof in the form of a solid together with water or as an aqueous slurry; b) dosing a peracid under stirring to the reaction mixture in an amount of 1.0 to 2.5 mol per mol of secondary amine; and c) isolating the organic phase.

    摘要翻译: 本发明涉及通过用有机过酸氧化从其相应的仲胺制备二级氮氧自由基的方法,包括以下步骤:a)向反应容器中加入仲胺,任选与有机溶剂一起加入一次 碱选自碱金属,碱土金属或碳酸氢铵,碱土金属或铵的碳酸盐或其混合物,其形式为水,或与水相混合; b)在搅拌下将过酸给予反应混合物,其量为每摩尔仲胺为1.0至2.5摩尔; 和c)分离有机相。

    Method for preparing &bgr;-phosphorous nitroxide radicals
    7.
    发明授权
    Method for preparing &bgr;-phosphorous nitroxide radicals 有权
    制备β-磷氮氧自由基的方法

    公开(公告)号:US06624322B1

    公开(公告)日:2003-09-23

    申请号:US09869911

    申请日:2001-11-09

    IPC分类号: C07F902

    CPC分类号: C07B61/02 C07F9/4006

    摘要: The invention concerns a method for preparing &bgr;-phosphorous nitroxide radicals which comprises preparing in a first step an aminophosphonate by reacting a carbonyl compound, a primary amine and a phosphorous compound, then in a second step in oxidizing said aminophosphonate using on-halogenated organic peracids in a two-phase organic water/solvent medium with a buffered aqueous phase with a pH ranging between 5 and 12.

    摘要翻译: 本发明涉及一种制备β-磷氮氧自由基的方法,其包括在第一步中通过使羰基化合物,伯胺和磷化合物反应制备氨基膦酸酯,然后在第二步中使用卤代有机过酸来氧化所述氨基膦酸酯 在具有pH在5和12之间的缓冲水相的两相有机水/溶剂介质中。

    SOLID-PHASE SUPPORT FOR OLIGONUCLEOTIDE SYNTHESIS AND OLIGONUCLEOTIDE SYNTHESIS METHOD
    9.
    发明申请
    SOLID-PHASE SUPPORT FOR OLIGONUCLEOTIDE SYNTHESIS AND OLIGONUCLEOTIDE SYNTHESIS METHOD 有权
    寡核苷酸合成和寡核苷酸合成方法的固相支持

    公开(公告)号:US20130317206A1

    公开(公告)日:2013-11-28

    申请号:US13901266

    申请日:2013-05-23

    IPC分类号: C08F22/10 C07H21/04

    摘要: The present invention provides a solid-phase support for oligonucleotide synthesis for synthesizing long chain oligonucleotide, RNA oligonucleotide and modified oligonucleotide at high synthetic quantity and high purity with a low loading amount of a linker. Provided is a solid-phase support for oligonucleotide synthesis comprising a porous resin bead having a monovinyl monomer unit, a crosslinkable vinyl monomer unit and a polyethylene glycol unit and a cleavable linker loaded on its surface, the porous resin bead having a group capable of binding to a carboxy group by a dehydration condensation reaction on its surface, the cleavable linker having a carboxy group, wherein the carboxy group of the cleavable linker is bound to the group capable of binding to a carboxy group, by a dehydration condensation reaction, and a loading amount of the cleavable linker is 1 to 80 μmol/g relative to the weight of the porous resin bead.

    摘要翻译: 本发明提供了一种用于合成高链寡核苷酸,RNA寡核苷酸和高合成量和高纯度的具有低负载量的接头的高纯度的修饰的寡核苷酸的寡核苷酸合成的固相支持物。 提供了一种用于寡核苷酸合成的固相载体,其包含具有单乙烯基单体单元,可交联乙烯基单体单元和聚乙二醇单元的多孔树脂珠粒和其表面上负载的可切割连接物,所述多孔树脂珠粒具有能够结合的基团 通过其表面上的脱水缩合反应与羧基反应,可切割接头具有羧基,其中可切割接头的羧基通过脱水缩合反应与能结合羧基的基团结合,并且 可切割接头的负载量相对于多孔树脂珠的重量为1〜80μmol/ g。