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公开(公告)号：US08232387B2
公开(公告)日：2012-07-31
申请号：US12857939
申请日：2010-08-17
申请人： Julian Paul Henschke , Xiaoheng Zhang , Guodong Chu , Lijun Mei , Yung Fa Chen
发明人： Julian Paul Henschke , Xiaoheng Zhang , Guodong Chu , Lijun Mei , Yung Fa Chen
CPC分类号： C07H19/173 , C07H1/00
摘要： A process for the preparation of cladribine of API grade is provided by direct coupling of O-protected 2-deoxy-ribofuranose with silylated 2-chloroadenine followed by deprotection of the resultant protected nucleoside in a separate step and then a purification step. Following the coupling, the desired N-9-glycosylated β-anomer of the nucleoside is directly isolated as a solid from the coupling reaction mixture by filtration in relatively high purity and yield, and it does not require purification.
摘要翻译： 通过将O-保护的2-脱氧 - 呋喃核糖与甲硅烷基化的2-氯腺嘌呤直接偶联，然后在单独的步骤中将所得的被保护的核苷脱保护，然后进行纯化步骤，提供API级克拉屈滨的制备方法。 偶联后，通过过滤以相对较高的纯度和产率将核苷的所需N-9-糖基化 - 单体直接从偶联反应混合物中分离为固体，并且不需要纯化。
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公开(公告)号：US20120197010A1
公开(公告)日：2012-08-02
申请号：US13429827
申请日：2012-03-26
申请人： Julian Paul HENSCHKE , Xiaoheng Zhang , Guodong Chu , Lijun Mei , Yung Fa Chen
发明人： Julian Paul HENSCHKE , Xiaoheng Zhang , Guodong Chu , Lijun Mei , Yung Fa Chen
IPC分类号： C07H1/06
CPC分类号： C07H19/173 , C07H1/00
摘要： A method of making cladribine with an increased purity comprising: a) dissolving crude cladribine in a protic solvent in the presence of a base to form a solution comprising dissolved crude cladribine; b) maintaining the solution at an elevated temperature so that the solution is homogeneous until the amount of protected or partially protected nucleoside impurities in the solution is reduced to a pre-determined upper limit; and c) cooling the solution of step b) so that crystals of cladribine are formed and isolated.
摘要翻译： 制备具有增加的纯度的克拉屈滨的方法包括：a）在碱存在下将粗克拉屈滨溶解在质子溶剂中以形成包含溶解的粗克拉屈滨的溶液; b）将溶液保持在升高的温度，使得溶液是均匀的，直到溶液中受保护或部分保护的核苷杂质的量减少到预定的上限; 和c）冷却步骤b）的溶液，使得克拉屈滨晶体形成和分离。
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公开(公告)号：US20110046363A1
公开(公告)日：2011-02-24
申请号：US12857939
申请日：2010-08-17
申请人： Julian Paul Henschke , Xiaoheng Zhang , Guodong Chu , Lijun Mei , Yung Fa Chen
发明人： Julian Paul Henschke , Xiaoheng Zhang , Guodong Chu , Lijun Mei , Yung Fa Chen
IPC分类号： C07H19/173
CPC分类号： C07H19/173 , C07H1/00
摘要： A process for the preparation of cladribine of API grade is provided by direct coupling of O-protected 2-deoxy-ribofuranose with silylated 2-chloroadenine followed by deprotection of the resultant protected nucleoside in a separate step and then a purification step. Following the coupling, the desired N-9-glycosylated β-anomer of the nucleoside is directly isolated as a solid from the coupling reaction mixture by filtration in relatively high purity and yield, and it does not require purification.
摘要翻译： 通过将O-保护的2-脱氧 - 呋喃核糖与甲硅烷基化的2-氯腺嘌呤直接偶联，然后在单独的步骤中将所得保护的核苷脱保护，然后进行纯化步骤，来提供制备API级克拉屈滨的方法。 偶联后，通过过滤以相对较高的纯度和产率将核苷的所需N-9-糖基化 - 单体直接从偶联反应混合物中分离为固体，并且不需要纯化。
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4.发明授权Preparation of 2-chloro-9-(2′-deoxy-2′-fluoro-β-D-arabinofuranosyl)-adenine 有权2-氯-9-（2'-脱氧-2'-氟-β-D-阿拉伯呋喃糖基） - 腺苷的制备公开(公告)号：US08648188B2
公开(公告)日：2014-02-11
申请号：US13179259
申请日：2011-07-08
申请人： Julian Paul Henschke , Xiaoheng Zhang , Lijun Mei , Yung-Fa Chen
发明人： Julian Paul Henschke , Xiaoheng Zhang , Lijun Mei , Yung-Fa Chen
CPC分类号： C07H19/167 , C07H19/19 , Y02P20/55
摘要： A process for making clofarabine comprising: fluorinating a compound of formula VII wherein each R4 is independently a hydroxy protecting group, OR6 is a leaving group, with a fluorinating agent in the presence of guanidine carbonate to give a compound of formula VIII: wherein R4 is as defined above; and deprotecting the compound of formula VIII to give the clofarabine.
摘要翻译： 制备氯法拉宾的方法，其包括：在碳酸胍存在下氟化式VII化合物，其中每个R 4独立地是羟基保护基，OR 6是离去基团，与氟化剂反应，得到式VIII化合物：其中R 4是 如上所述; 并使式VIII的化合物脱保护得到氯法拉滨。
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5.发明申请Preparation of 2-chloro-9-(2'-deoxy-2'-fluoro-Beta-D-arabinofuranosyl)-adenine 有权2-氯-9-（2'-脱氧-2'-氟-β-D-阿拉伯呋喃糖基） - 腺苷的制备公开(公告)号：US20120010397A1
公开(公告)日：2012-01-12
申请号：US13179259
申请日：2011-07-08
申请人： Julian Paul Henschke , Xiaoheng Zhang , Lijun Mei , Yung-Fa Chen
发明人： Julian Paul Henschke , Xiaoheng Zhang , Lijun Mei , Yung-Fa Chen
IPC分类号： C07H19/16
CPC分类号： C07H19/167 , C07H19/19 , Y02P20/55
摘要： A process for making clofarabine comprising: fluorinating a compound of formula VII wherein each R4 is independently a hydroxy protecting group, OR6 is a leaving group, with a fluorinating agent in the presence of guanidine carbonate to give a compound of formula VIII: wherein R4 is as defined above; and deprotecting the compound of formula VIII to give the clofarabine.
摘要翻译： 制备氯法拉宾的方法，其包括：在碳酸胍存在下氟化式VII化合物，其中每个R 4独立地是羟基保护基，OR 6是离去基团，与氟化剂反应，得到式VIII化合物：其中R 4是 如上所述; 并使式VIII的化合物脱保护得到氯法拉滨。
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公开(公告)号：US08338586B2
公开(公告)日：2012-12-25
申请号：US13429827
申请日：2012-03-26
申请人： Julian Paul Henschke , Xiaoheng Zhang , Chu Guodong , Lijun Mei , Yung Fa Chen
发明人： Julian Paul Henschke , Xiaoheng Zhang , Chu Guodong , Lijun Mei , Yung Fa Chen
CPC分类号： C07H19/173 , C07H1/00
摘要： A method of making cladribine with an increased purity comprising: a) dissolving crude cladribine in a protic solvent in the presence of a base to form a solution comprising dissolved crude cladribine; b) maintaining the solution at an elevated temperature so that the solution is homogeneous until the amount of protected or partially protected nucleoside impurities in the solution is reduced to a pre-determined upper limit; and c) cooling the solution of step b) so that crystals of cladribine are formed and isolated.
摘要翻译： 制备具有增加的纯度的克拉屈滨的方法包括：a）在碱存在下将粗克拉屈滨溶解在质子溶剂中以形成包含溶解的粗克拉屈滨的溶液; b）将溶液保持在升高的温度，使得溶液是均匀的，直到溶液中受保护或部分保护的核苷杂质的量减少到预定的上限; 和c）冷却步骤b）的溶液，使得克拉屈滨晶体形成和分离。
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公开(公告)号：US20100087637A1
公开(公告)日：2010-04-08
申请号：US12572578
申请日：2009-10-02
申请人： Julian Paul Henschke , Xiaoheng Zhang , Jianbo Yu , Kun Hu , Lijun Mei
发明人： Julian Paul Henschke , Xiaoheng Zhang , Jianbo Yu , Kun Hu , Lijun Mei
IPC分类号： C07H19/12
摘要： A method for producing a β-enriched protected decitabine comprising: a) coupling a protected 2-deoxy-ribofuranose with a protected 5-azacytosine in the presence of a catalyst to form a reaction mixture comprising the protected decitabine of formula I; and b) quenching the reaction mixture of step a) with a base. The β-enriched protected decitabine so made may be deprotected to produce a decitabine product in a high yield and purity.
摘要翻译： 一种生产富集的受保护的地西他滨的方法，包括：a）在催化剂存在下将受保护的2-脱氧 - 呋喃核糖与受保护的5-氮杂胞嘧啶偶联，形成包含式I的受保护的地西他滨的反应混合物; 和b）将碱的步骤a）的反应混合物淬灭。 如此制备的富含生物保护的地西他滨可以去保护以产生高产率和纯度的地西他滨产品。
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公开(公告)号：US08586729B2
公开(公告)日：2013-11-19
申请号：US12572578
申请日：2009-10-02
申请人： Julian Paul Henschke , Xiaoheng Zhang , Jianbo Yu , Kun Hu , Lijun Mei
发明人： Julian Paul Henschke , Xiaoheng Zhang , Jianbo Yu , Kun Hu , Lijun Mei
摘要： A method for producing a β-enriched protected decitabine comprising: a) coupling a protected 2-deoxy-ribofuranose with a protected 5-azacytosine in the presence of a catalyst to form a reaction mixture comprising the protected decitabine of formula I; and b) quenching the reaction mixture of step a) with a base. The β-enriched protected decitabine so made may be deprotected to produce a decitabine product in a high yield and purity.
摘要翻译： 一种制备富含β-的受保护的地西他滨的方法，包括：a）在催化剂存在下将受保护的2-脱氧 - 呋喃核糖与受保护的5-氮杂胞嘧啶偶联，形成包含式I的受保护的地西他滨的反应混合物; 和b）将碱的步骤a）的反应混合物淬灭。 如此制备的β-富集的保护的地西他滨可以去保护以产生高产率和纯度的地西他滨产品。
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