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1. 发明申请

WO2007134160A2 TEMPERATURE-JUMP DYNAMIC NUCLEAR POLARIZATION 审中-公开
标题翻译：温度 - 跳动动态核极化
公开(公告)号：WO2007134160A2
公开(公告)日：2007-11-22
申请号：PCT/US2007/068654
申请日：2007-05-10
申请人： MASSACHUSETTS INSTITUTE OF TECHNOLOGY , GRIFFIN, Robert, G. , HU, Kan-Nian , JOO, Chan, Gyu
发明人： GRIFFIN, Robert, G. , HU, Kan-Nian , JOO, Chan, Gyu
IPC分类号： G06Q30/00
CPC分类号： G01R33/62 , G01N24/08 , G01N24/087 , G01N24/10 , G01R33/282 , G01R33/30 , G01R33/46
摘要： In one aspect, the present invention provides a method for enhancing the sensitivity of liquid- state NMR or MRI experiments. In general, the method involves (a) providing a frozen sample in a magnetic field, wherein the frozen sample includes a polarizing agent with at least one unpaired electron and an analyte with at least one spin half nucleus; (b) polarizing the at least one spin half nucleus of the analyte by irradiating the frozen sample with radiation having a frequency that excites electron spin transitions in the at least one unpaired electron of the polarizing agent; (c) melting the frozen sample to produce a molten sample; and (d) detecting nuclear spin transitions in the at least one spin half nucleus of the analyte in the molten sample. In certain embodiments, the methods further comprise a step of freezing a sample in a magnetic field to provide the frozen sample in a magnetic field. The freezing, polarizing, melting and detecting steps may be repeated as many times as desired. In another aspect, the present invention provides systems for performing these methods.
摘要翻译：一方面，本发明提供了一种提高液态NMR或MRI实验灵敏度的方法。通常，该方法包括（a）在磁场中提供冷冻样品，其中冷冻样品包括具有至少一个不成对电子的偏振剂和具有至少一个旋转半核的分析物; （b）通过用具有激发所述至少一种不成对的电子中的电子自旋跃迁的频率的辐射照射所述冷冻样品来使所述分析物的所述至少一个旋转半核偏振; （c）熔化冷冻样品以产生熔融样品; 和（d）检测熔融样品中分析物的至少一个旋转半核中的核自旋跃迁。在某些实施方案中，所述方法还包括在磁场中冷冻样品以在磁场中提供冷冻样品的步骤。冷冻，极化，熔化和检测步骤可以根据需要重复多次。在另一方面，本发明提供了用于执行这些方法的系统。

2. 发明申请

WO2008048714A2 BIRADICAL POLARIZING AGENTS FOR DYNAMIC NUCLEAR POLARIZATION 审中-公开
标题翻译：用于动态核极化的双极化极化剂
公开(公告)号：WO2008048714A2
公开(公告)日：2008-04-24
申请号：PCT/US2007068659
申请日：2007-05-10
申请人： MASSACHUSETTS INST TECHNOLOGY , GRIFFIN ROBERT G , HU KAN-NIAN , SWAGER TIMOTHY M , SONG CHANGSIK , DANE ERIC
发明人： GRIFFIN ROBERT G , HU KAN-NIAN , SWAGER TIMOTHY M , SONG CHANGSIK , DANE ERIC
IPC分类号： G01N24/08
CPC分类号： G01R33/281 , C07D401/12 , G01N24/087 , G01R33/465 , G01R33/5601 , Y10T436/24
摘要： The present invention provides methods for performing dynamic nuclear polarization using biradicals with a structure of formula (I) as described herein. In general, the methods involve (a) providing a frozen sample in a magnetic field, wherein the frozen sample includes a biradical of formula (I) and an analyte with at least one spin half nucleus; (b) polarizing the at least one spin half nucleus of the analyte by irradiating the frozen sample with radiation having a frequency that excites electron spin transitions in the biradical; (c) optionally melting the sample to produce a molten sample; and (d) detecting nuclear spin transitions in the at least one spin half nucleus of the analyte in the frozen or molten sample. The present invention also provides biradicals with a structure of formula (I) with the proviso that Q 1 and Q 2 are different when X 1 and X 2 are -O-. The present invention also provides methods for making biradicals with a structure of formula (IA) as described herein.
摘要翻译：本发明提供使用如本文所述的式（I）结构的双基进行动态核极化的方法。通常，所述方法包括（a）在磁场中提供冷冻样品，其中所述冷冻样品包括式（I）的双基和具有至少一个自旋半核的分析物; （b）通过用具有激发双向电子自旋跃迁的频率的辐射照射冷冻样品来使分析物的至少一个自旋半核偏振; （c）任选地熔化样品以产生熔融样品; 和（d）检测冷冻或熔融样品中分析物的至少一个旋转半核中的核自旋跃迁。本发明还提供了具有式（I）结构的双基，条件是当X 1和X 2独立地相同时，Q 1和Q 2 2不同 X 2是-O-。本发明还提供了如本文所述制备具有式（IA）结构的双基质的方法。

3. 发明申请

WO2007134160A3 TEMPERATURE-JUMP DYNAMIC NUCLEAR POLARIZATION 审中-公开
标题翻译：温度 - 跳动动态核极化
公开(公告)号：WO2007134160A3
公开(公告)日：2008-04-24
申请号：PCT/US2007068654
申请日：2007-05-10
申请人： MASSACHUSETTS INST TECHNOLOGY , GRIFFIN ROBERT G , HU KAN-NIAN , JOO CHAN GYU
发明人： GRIFFIN ROBERT G , HU KAN-NIAN , JOO CHAN GYU
IPC分类号： G01R33/46
CPC分类号： G01R33/62 , G01N24/08 , G01N24/087 , G01N24/10 , G01R33/282 , G01R33/30 , G01R33/46
摘要： In one aspect, the present invention provides a method for enhancing the sensitivity of liquid-state NMR or MRI experiments. In general, the method involves providing a frozen sample in a magnetic field, wherein the frozen sample includes a polarizing agent with at least one unpaired electron and an analyte with at least one spin half nucleus; polarizing the at least one spin half nucleus of the analyte by irradiating the frozen sample with radiation having a frequency that excites electron spin transitions in the at least one unpaired electron of the polarizing agent; melting the frozen sample to produce a molten sample; and (d) detecting nuclear spin transitions in the at least one spin half nucleus of the analyte in the molten sample. In certain embodiments, the methods further comprise a step of freezing a sample in a magnetic field to provide the frozen sample in a magnetic field.
摘要翻译：一方面，本发明提供了提高液态NMR或MRI实验的灵敏度的方法。通常，该方法包括在磁场中提供冷冻样品，其中冷冻样品包括具有至少一个不成对电子的偏振剂和具有至少一个旋转半核的分析物; 通过用具有激发所述至少一个非配对电子中的电子自旋跃迁的频率的辐射照射所述冷冻样品来使所述分析物的至少一个旋转半核偏振; 熔化冷冻样品以产生熔融样品; 和（d）检测熔融样品中分析物的至少一个自旋半核中的核自旋跃迁。在某些实施方案中，所述方法还包括在磁场中冷冻样品以在磁场中提供冷冻样品的步骤。

4. 发明申请

WO2005024440A3 POLARIZING AGENTS FOR DYNAMIC NUCLEAR POLARIZATION 审中-公开
公开(公告)号：WO2005024440A3
公开(公告)日：2005-03-17
申请号：PCT/US2004/026968
申请日：2004-08-19
申请人： MASSACHUSETTS INSTITUTE OF TECHNOLOGY , GRIFFIN, Robert, G. , HU, Kan-Nian
发明人： GRIFFIN, Robert, G. , HU, Kan-Nian
IPC分类号： A61B5/055 , A61K49/00
摘要： We describe polarizing agents for use in enhancing NMR and MRI signals via dynamic nuclear polarization (DNP). The polarizing agents include two or more paramagnetic centers, preferably two paramagnetic centers. In a preferred embodiment, the polarizing agent comprises two nitroxide radicals tethered by a polyethylene glycol chain of variable length. Signal enhancements of up to 175 have been achieved in comparison with factors of ~45 at similar concentrations of monomeric radical such as TEMPO.

5. 发明申请

WO2013016490A1 THIOPHENE COMPOUNDS 审中-公开
标题翻译：噻吩化合物
公开(公告)号：WO2013016490A1
公开(公告)日：2013-01-31
申请号：PCT/US2012/048258
申请日：2012-07-26
申请人： VERTEX PHARMACEUTICALS INCORPORATED , LUISI, Brian , WILLCOX, David , ROEPER, Stefanie , HU, Kan-Nian , LUONG, Hoa, Q.
发明人： LUISI, Brian , WILLCOX, David , ROEPER, Stefanie , HU, Kan-Nian , LUONG, Hoa, Q.
IPC分类号： C07D333/40 , A61K31/381 , A61P31/14
CPC分类号： C07D333/40 , A61K9/0019 , A61K9/1652 , A61K9/2054 , A61K9/2077 , A61K9/4858 , A61K9/4866 , A61K31/381 , A61K47/40 , C07D333/38
摘要： Polymorph Forms M, H, P, X, and ZA of Compound (1) represented by the following structural formula: are described. A method of preparing polymorph Form M of Compound (1) includes stirring a mixture of Compound (1) and a solvent system that includes isopropanol, ethyl acetate, n -butyl acetate, methyl acetate, acetone, 2-butanone (methylethylketone (MEK)), or heptane, or a combination thereof at a temperature in a range of 10 °C to 47 °C to form From M of Compound (1). A method of preparing polymorph Form H of Compound (1) includes stirring a solution of Compound (1) at a temperature in a range of 48 °C to 70 °C to form Form H of Compound (1). A method of preparing polymorph Form P of Compound (1) includes stirring a mixture of Compound (1) and a solvent system that includes a solvent selected from the group consisting of dichloromethane and tetrahydrofuran (THF), and a mixture thereof at room temperature to form Form P of Compound (1). A method of preparing polymorph Form X of Compound (1) includes removing ethyl acetate from ethylacetate solvate G of Compound (1). A method of preparing polymorph Form ZA of Compound (1) includes removing n -butyl acetate from n-butyl acetate solvate A of Compound (1).
摘要翻译：描述了由以下结构式表示的化合物（1）的多晶型：M，H，P，X和ZA。制备化合物（1）的多晶型物M的方法包括搅拌化合物（1）和包括异丙醇，乙酸乙酯，乙酸正丁酯，乙酸甲酯，丙酮，2-丁酮（甲基乙基酮（MEK））的溶剂体系的混合物，）或庚烷或其组合，在10℃至47℃的温度范围内，以形成化合物（1）的M。制备化合物（1）的多晶型物H的方法包括在48℃至70℃的温度范围内搅拌化合物（1）的溶液以形成化合物（1）的H型。制备化合物（1）的多晶型P的方法包括：将化合物（1）和包含选自二氯甲烷和四氢呋喃（THF）的溶剂的溶剂体系的混合物及其混合物在室温下搅拌至形成化合物（1）的形式P. 制备化合物（1）的多晶型物X的方法包括从化合物（1）的乙酸乙酯溶剂化物G中除去乙酸乙酯。制备化合物（1）的多晶型ZA的方法包括从化合物（1）的乙酸正丁酯溶剂化物A中除去乙酸正丁酯。

6. 发明申请

WO2008048714A3 BIRADICAL POLARIZING AGENTS FOR DYNAMIC NUCLEAR POLARIZATION 审中-公开
公开(公告)号：WO2008048714A3
公开(公告)日：2008-04-24
申请号：PCT/US2007/068659
申请日：2007-05-10
申请人： MASSACHUSETTS INSTITUTE OF TECHNOLOGY , GRIFFIN, Robert, G. , HU, Kan-Nian , SWAGER, Timothy, M , SONG, Changsik , DANE, Eric
发明人： GRIFFIN, Robert, G. , HU, Kan-Nian , SWAGER, Timothy, M , SONG, Changsik , DANE, Eric
IPC分类号： G01N24/12 , A01N43/40 , C07D207/46 , C07D419/12
摘要： The present invention provides biradicals with a structure of formula (I) and methods for performing dynamic nuclear polarization using the biradicals. The methods involve (a) providing a fro∑en sample in a magnetic field, the frozen sample including a biradical of formula (1) and an analyte with at least one spin half nucleus; (b) polarizing the at least one spin half nucleus of the analyte by irradiating the frozen sample with radiation haviig a frequency that excites electron spin transitions in the biradical; (c) optionally melting the sample to produce a molten sample; and (d) detecting nuclear spin transitions in the at least one spin half nucleus of the analyte in the. The present inventon also provides methods for making biradicals with a structure of formula (IA).

7. 发明申请

WO2005024440A2 POLARIZING AGENTS FOR DYNAMIC NUCLEAR POLARIZATION 审中-公开
标题翻译：用于动态核极化的极化剂
公开(公告)号：WO2005024440A2
公开(公告)日：2005-03-17
申请号：PCT/US2004026968
申请日：2004-08-19
申请人： MASSACHUSETTS INST TECHNOLOGY , GRIFFIN ROBERT G , HU KAN-NIAN
发明人： GRIFFIN ROBERT G , HU KAN-NIAN
IPC分类号： A61B5/05 , A61B5/055 , C07D409/14 , G01R20060101 , G01R33/28 , G01R33/60 , G01R
CPC分类号： G01R33/282 , C07D409/14 , G01R33/5601 , G01R33/60 , Y10T436/24
摘要： We describe polarizing agents for use in enhancing NMR and MRI signals via dynamic nuclear polarization (DNP). The polarizing agents include two or more paramagnetic centers, preferably two paramagnetic centers. In a preferred embodiment, the polarizing agent comprises two nitroxide radicals tethered by a polyethylene glycol chain of variable length. Signal enhancements of up to 175 have been achieved in comparison with factors of ~45 at similar concentrations of monomeric radical such as TEMPO.
摘要翻译：我们描述了通过动态核极化（DNP）增强核磁共振和核磁共振信号的极化剂。偏振剂包括两个或更多个顺磁中心，优选两个顺磁中心。在优选的实施方案中，偏振剂包含由可变长度的聚乙二醇链束缚的两个氮氧自由基。与类似浓度的单体自由基（如TEMPO）相比，可以达到高达175的信号增强。

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