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    Process for preparation of isosulfan blue
    2.
    发明授权
    Process for preparation of isosulfan blue 有权
    制备异硫丹蓝的方法

    公开(公告)号：US07662992B2

    公开(公告)日：2010-02-16

    申请号：US12180057

    申请日：2008-07-25

    申请人： Ravishanker Kovi ,  Satyam Nampalli ,  Peter Xavier Tharial

    发明人： Ravishanker Kovi ,  Satyam Nampalli ,  Peter Xavier Tharial

    IPC分类号： C07C309/00

    CPC分类号： C07C309/46 ,  C07C303/02 ,  C07C303/22 ,  C07C309/52

    摘要： A process for the preparation of isosulfan blue (Active Pharmaceutical Ingredient) is provided. A process is also provided for preparation of the intermediate, 2-chlorobenzaldehyde-5-sulfonic acid, sodium salt of formula (2), used in the preparation thereof and a procedure for the isolation of benzaldehyde-2,5-disulfonic acid, di-sodium salt of the formula (3). Also provided is a process for the preparation of an isoleuco acid of formula (4), which upon mild oxidation gives rise to isosulfan blue of pharmaceutical grade which can be used for preparation of pharmaceutical formulations. The isolation and purification procedures provided in the process provide substantially pure isosulfan blue with HPLC purity 99.5% or greater.

    摘要翻译： 提供了制备异硫丹蓝（Active Pharmaceutical Ingredient）的方法。 还提供了制备用于其制备的中间体2-氯苯甲醛-5-磺酸，式（2）的钠盐的方法和用于分离苯甲醛-2,5-二磺酸，二 式（3）的钠盐。 还提供了制备式（4）的异亮氨酸的方法，其在轻微氧化时产生可用于制备药物制剂的药物级别的异硫丹蓝。 该方法中提供的分离和纯化方法提供基本上纯的异硫丹蓝，HPLC纯度为99.5％或更高。

    Process for preparation of 5H-dibenzo[a,d] cycloheptene derivatives
    3.
    发明授权
    Process for preparation of 5H-dibenzo[a,d] cycloheptene derivatives 有权
    制备5H-二苯并[a，d]环庚烯衍生物的方法

    公开(公告)号：US07446227B2

    公开(公告)日：2008-11-04

    申请号：US11609075

    申请日：2006-12-11

    申请人： Satyam Nampalli ,  Brijesh Patel ,  Peter Xavier Tharial ,  Ravishanker Kovi

    发明人： Satyam Nampalli ,  Brijesh Patel ,  Peter Xavier Tharial ,  Ravishanker Kovi

    IPC分类号： C07C211/00

    CPC分类号： C07C29/32 ,  C07C209/22 ,  C07C303/28 ,  C07C2603/32 ,  C07C211/32 ,  C07C309/66 ,  C07C33/38

    摘要： A process for preparation of protriptyline hydrochloride from 5-dihydrobenzocycloheptatriene of formula (1) by coupling with chloropropyl alcohol in the presence of excess n-butyl Lithium in tetrahydrofuran under inert atmosphere, followed by preparation of mesylate derivative of formula (3) and finally the nucleophilic displacement of the mesylate group by reacting methylamine solution in methanol to give protriptyline free base of the formula (4). Also the present process reveals the hydrochloride salt formation and purification of the same to give pure pharmaceutical grade protriptyline hydrochloride with impurities less than 0.1% w/w.

    摘要翻译： 在惰性气氛下，在四氢呋喃中，在过量的正丁基锂存在下，用氯丙醇与氯丙醇偶合制备式（1）的5-二氢苯并环庚三烯的方法，然后制备式（3）的甲磺酸酯衍生物， 通过使甲胺溶液在甲醇中反应，得到式（4）的无游离碱，从而亲核取代甲磺酸酯基。 此外，本发明方法显示盐酸盐形成和纯化，得到纯度为0.1％w / w的杂质的药物级羟基替康林盐酸盐。

    PROCESS FOR PREPARATION OF 5H-DIBENZO[A,D] CYCLOHEPTENE DERIVATIVES
    4.
    发明申请
    PROCESS FOR PREPARATION OF 5H-DIBENZO[A,D] CYCLOHEPTENE DERIVATIVES 有权
    制备5H-二苯并[A，D]环己基衍生物的方法

    公开(公告)号：US20080139848A1

    公开(公告)日：2008-06-12

    申请号：US11609075

    申请日：2006-12-11

    申请人： Satyam S. Nampalli ,  Brijesh Patel ,  Peter Xavier Tharial ,  Ravishanker Kovi

    发明人： Satyam S. Nampalli ,  Brijesh Patel ,  Peter Xavier Tharial ,  Ravishanker Kovi

    IPC分类号： C07C33/16 ,  C07C211/31

    CPC分类号： C07C29/32 ,  C07C209/22 ,  C07C303/28 ,  C07C2603/32 ,  C07C211/32 ,  C07C309/66 ,  C07C33/38

    摘要： A process for preparation of protriptyline hydrochloride from 5-dihydrobenzocycloheptatriene of formula (1) by coupling with chloropropyl alcohol in the presence of excess n-butyl Lithium in tetrahydrofuran under inert atmosphere, followed by preparation of mesylate derivative of formula (3) and finally the nucleophilic displacement of the mesylate group by reacting methylamine solution in methanol to give protriptyline free base of the formula (4). Also the present process reveals the hydrochloride salt formation and purification of the same to give pure pharmaceutical grade protriptyline hydrochloride with impurities less than 0.1% w/w.

    摘要翻译： 在惰性气氛下，在四氢呋喃中，在过量的正丁基锂存在下，用氯丙醇与氯丙醇偶合制备式（1）的5-二氢苯并环庚三烯的方法，然后制备式（3）的甲磺酸酯衍生物， 通过使甲胺溶液在甲醇中反应，得到式（4）的无游离碱，从而亲核取代甲磺酸酯基。 此外，本发明方法显示盐酸盐形成和纯化，得到纯度为0.1％w / w的杂质的药物级羟基替康林盐酸盐。

    PROCESS FOR PREPARATION ISOSULFAN BLUE
    7.
    发明申请
    PROCESS FOR PREPARATION ISOSULFAN BLUE 有权
    制备ISOSULFAN蓝色的方法

    公开(公告)号：US20080293963A1

    公开(公告)日：2008-11-27

    申请号：US12180057

    申请日：2008-07-25

    申请人： Ravishanker Kovi ,  Satyam Nampalli ,  Peter Xavier Tharial

    发明人： Ravishanker Kovi ,  Satyam Nampalli ,  Peter Xavier Tharial

    IPC分类号： C07C309/46 ,  C07C309/44

    CPC分类号： C07C309/46 ,  C07C303/02 ,  C07C303/22 ,  C07C309/52

    摘要： A process for the preparation of isosulfan blue (Active Pharmaceutical Ingredient) is provided. A process is also provided for preparation of the intermediate, 2-chlorobenzaldehyde-5-sulfonic acid, sodium salt of formula (2), used in the preparation thereof and a procedure for the isolation of benzaldehyde-2,5-disulfonic acid, di-sodium salt of the formula (3). Also provided is a process for the preparation of an isoleuco acid of formula (4), which upon mild oxidation gives rise to isosulfan blue of pharmaceutical grade which can be used for preparation of pharmaceutical formulations. The isolation and purification procedures provided in the process provide substantially pure isosulfan blue with HPLC purity 99.5% or greater.

    摘要翻译： 提供了制备异硫丹蓝（Active Pharmaceutical Ingredient）的方法。 还提供了制备用于其制备的中间体2-氯苯甲醛-5-磺酸，式（2）的钠盐的方法和用于分离苯甲醛-2,5-二磺酸，二 式（3）的钠盐。 还提供了制备式（4）的异亮氨酸的方法，其在轻微氧化时产生可用于制备药物制剂的药物级别的异硫丹蓝。 该方法中提供的分离和纯化方法提供基本上纯的异硫丹蓝，HPLC纯度为99.5％或更高。

    PROCESS FOR PREPARATION OF ISOSULFAN BLUE
    8.
    发明申请
    PROCESS FOR PREPARATION OF ISOSULFAN BLUE 有权
    制备ISOSULFAN蓝的方法

    公开(公告)号：US20130310600A1

    公开(公告)日：2013-11-21

    申请号：US13951034

    申请日：2013-07-25

    申请人： Ravishanker Kovi ,  Satyam Nampalli ,  Peter Xavier Tharial

    发明人： Ravishanker Kovi ,  Satyam Nampalli ,  Peter Xavier Tharial

    IPC分类号： C07C303/02

    CPC分类号： C07C309/46 ,  C07C303/02 ,  C07C303/22 ,  C07C309/52

    摘要： A process for the preparation of isosulfan blue (Active Pharmaceutical Ingredient) is provided. A process is also provided for preparation of the intermediate, 2-chlorobenzaldehyde-5-sulfonic acid, sodium salt of formula (2), used in the preparation thereof and a procedure for the isolation of benzaldehyde-2,5-disulfonic acid, di-sodium salt of the formula (3). Also provided is a process for the preparation of an isoleuco acid of formula (4), which upon mild oxidation gives rise to isosulfan blue of pharmaceutical grade which can be used for preparation of pharmaceutical formulations. The isolation and purification procedures provided in the process provide substantially pure isosulfan blue with HPLC purity 99.5% or greater.

    摘要翻译： 提供了制备异硫丹蓝（Active Pharmaceutical Ingredient）的方法。 还提供了制备用于其制备的中间体2-氯苯甲醛-5-磺酸，式（2）的钠盐的方法和用于分离苯甲醛-2,5-二磺酸，二 式（3）的钠盐。 还提供了制备式（4）的异亮氨酸的方法，其在轻微氧化时产生可用于制备药物制剂的药物级别的异硫丹蓝。 该方法中提供的分离和纯化方法提供基本上纯的异硫丹蓝，HPLC纯度为99.5％或更高。

    Process for the preparation of cis-2-methylspiro (1,3-oxathiolane 5-3′) quinuclidine
    9.
    发明授权
    Process for the preparation of cis-2-methylspiro (1,3-oxathiolane 5-3′) quinuclidine 有权
    顺式-2-甲基螺（1,3-氧硫杂环戊烷-5- 3'）奎宁环的制备方法

    公开(公告)号：US08450487B2

    公开(公告)日：2013-05-28

    申请号：US12796308

    申请日：2010-06-08

    申请人： Ravishanker Kovi ,  Jayaraman Kannapan ,  Talluri Buhshaiah Chowdari ,  Chirag Vasantlal Shah

    发明人： Ravishanker Kovi ,  Jayaraman Kannapan ,  Talluri Buhshaiah Chowdari ,  Chirag Vasantlal Shah

    IPC分类号： C07D453/00

    CPC分类号： C07D497/20 ,  C07D453/04

    摘要： Methods are provided for making pharmaceutical-grade cis-2-methylspiro(1,3-oxathiolane-5,3′)quinuclidine and pharmaceutically acceptable salts thereof by isomerizing racemic 2-methylspiro(1,3-oxathiolane-5,3′)quinuclidine to cis-2-methylspiro(1,3-oxathiolane-5,3′)quinuclidine and subsequent purification of the C-MSOQ by salt formation with inexpensive and commercially available material such as sulfuric acid. Purification methods are disclosed which employ an organic solvent/water system and recrystallization with an organic solvent such as acetone.

    摘要翻译： 提供了通过将外消旋2-甲基螺（1,3-氧硫杂环戊烷-5,3'）奎宁环异构化制备药学级顺式-2-甲基螺（1,3-氧硫杂环戊烷-5,3'）奎宁环及其药学上可接受的盐的方法 顺式-2-甲基螺（1,3-氧硫杂环戊烷-5,3'）奎宁环，随后用便宜且市售的材料如硫酸通过盐形成纯化C-MSOQ。 公开了使用有机溶剂/水体系并用有机溶剂如丙酮重结晶的纯化方法。

    PROCESS FOR PREPARATION OF ISOSULFAN BLUE
    10.
    发明申请
    PROCESS FOR PREPARATION OF ISOSULFAN BLUE 审中-公开
    制备ISOSULFAN蓝的方法

    公开(公告)号：US20100094044A1

    公开(公告)日：2010-04-15

    申请号：US12643056

    申请日：2009-12-21

    申请人： RAVISHANKER KOVI ,  SATYAM NAMPALLI ,  PETER XAVIER THARIAL

    发明人： RAVISHANKER KOVI ,  SATYAM NAMPALLI ,  PETER XAVIER THARIAL

    IPC分类号： C07C309/29

    CPC分类号： C07C309/46 ,  C07C303/02 ,  C07C303/22 ,  C07C309/52

    摘要： A process for the preparation of isosulfan blue (Active Pharmaceutical Ingredient) is provided. A process is also provided for preparation of the intermediate, 2-chlorobenzaldehyde-5-sulfonic acid, sodium salt of formula (2), used in the preparation thereof and a procedure for the isolation of benzaldehyde-2,5-disulfonic acid, di-sodium salt of the formula (3). Also provided is a process for the preparation of an isoleuco acid of formula (4), which upon mild oxidation gives rise to isosulfan blue of pharmaceutical grade which can be used for preparation of pharmaceutical formulations. The isolation and purification procedures provided in the process provide substantially pure isosulfan blue with HPLC purity 99.5% or greater.

    摘要翻译： 提供了制备异硫丹蓝（Active Pharmaceutical Ingredient）的方法。 还提供了制备用于其制备的中间体2-氯苯甲醛-5-磺酸，式（2）的钠盐的方法和用于分离苯甲醛-2,5-二磺酸，二 式（3）的钠盐。 还提供了制备式（4）的异亮氨酸的方法，其在轻微氧化时产生可用于制备药物制剂的药物级别的异硫丹蓝。 该方法中提供的分离和纯化方法提供基本上纯的异硫丹蓝，HPLC纯度为99.5％或更高。