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    Synthesis of thiazole derivatives
    1.
    发明授权
    Synthesis of thiazole derivatives 失效
    噻唑衍生物的合成

    公开(公告)号：US5856501A

    公开(公告)日：1999-01-05

    申请号：US989096

    申请日：1997-12-11

    申请人： Arcelio J. Malcolm ,  Tse-Chong Wu

    发明人： Arcelio J. Malcolm ,  Tse-Chong Wu

    IPC分类号： C07D277/38 ,  C07D277/46 ,  C07D277/48

    CPC分类号： C07D277/48

    摘要： N-�4-(cyanoethylthiomethyl)-2-thiazolyl!guanidine--a key intermediate for preparing the pharmaceutical, famotidine--is produced by mixing in a liquid medium formed from a chemically indifferent organic solvent and water, and under an inert atmosphere, (i) a 2-guanidino-4-halomethylthiazole or a hydrohalide complex thereof, (ii) an S-(2-cyanoethyl)isothiourea or a hydrohalide complex thereof, and (iii) a strong alkali metal base. In lieu of (ii), an alkali metal salt of 2-cyanoethyl-1-thiol can be used, and in such case use of (iii) is optional, but preferable.

    摘要翻译： N- [4-（氰基乙硫基甲基）-2-噻唑基]胍 - 用于制备药物法莫替丁的关键中间体 - 通过在由化学无关的有机溶剂和水形成的液体介质中混合，并在惰性气氛下， i）2-胍基-4-卤代甲基噻唑或其氢卤化物络合物，（ii）S-（2-氰基乙基）异硫脲或其氢卤化物络合物，和（iii）强碱金属碱。 代替（ii），可以使用2-氰基乙基-1-硫醇的碱金属盐，在这种情况下，使用（iii）是任选的，但优选。

    Synthesis of thiazole derivatives
    2.
    发明授权
    Synthesis of thiazole derivatives 失效

    公开(公告)号：US5731442A

    公开(公告)日：1998-03-24

    申请号：US816111

    申请日：1997-03-11

    申请人： Arcelio J. Malcolm ,  Tse-Chong Wu

    发明人： Arcelio J. Malcolm ,  Tse-Chong Wu

    IPC分类号： C07D277/38 ,  C07D277/46 ,  C07D277/48

    CPC分类号： C07D277/48

    摘要： N-�4-(cyanoethylthiomethyl)-2-thiazolyl!guanidine--a key intermediate for preparing the pharmaceutical, famotidine--is produced by mixing in a liquid medium formed from a chemically indifferent organic solvent and water, and under an inert atmosphere, (i) a 2-guanidino-4-halomethylthiazole or a hydrohalide complex thereof, (ii) an S-(2-cyanoethyl)isothiourea or a hydrohalide complex thereof, and (iii) a strong alkali metal base. In lieu of (ii), an alkali metal salt of 2-cyanoethyl-1-thiol can be used, and in such case use of (iii) is optional, but preferable.

    Process for purifying neomenthyldiphenylphosphine using methanol
    3.
    发明授权
    Process for purifying neomenthyldiphenylphosphine using methanol 失效
    使用甲醇净化新戊基二苯基膦的方法

    公开(公告)号：US5994587A

    公开(公告)日：1999-11-30

    申请号：US84623

    申请日：1998-05-26

    申请人： Tse-Chong Wu ,  K. Pushpananda A. Senaratne

    发明人： Tse-Chong Wu ,  K. Pushpananda A. Senaratne

    IPC分类号： C07F9/50

    CPC分类号： C07F9/5095

    摘要： A process for the purification of crude neomenthyldiphenylphosphine, the process comprising crystallizing the crude neomenthyldiphenylphosphine using a solvent consisting essentially of methanol. The process provides for the unexpectedly efficient production of neomenthyldiphenylphosphine having purities of at least 97 mole percent, and more preferably at least about 99 mole percent. Another embodiment of the invention is neomenthyldiphenylphosphine having a purity of at least 97 mole percent produced by crystallizing crude neomenthyldiphenylphosphine having a purity of less than 97 mole percent using a solvent consisting essentially of methanol.

    摘要翻译： 一种用于纯化新戊基二苯基膦的方法，该方法包括使用基本上由甲醇组成的溶剂使粗新戊基二苯基膦结晶。 该方法提供意想不到的高效生产纯度至少为97摩尔％，更优选至少约99摩尔％的新戊基二苯基膦。 本发明的另一个实施方案是通过使用基本上由甲醇组成的溶剂，使纯度小于97摩尔％的粗新戊基二苯基膦结晶，得到纯度为至少97摩尔％的新戊基二苯基膦。

    PROCESS FOR MANUFACTURING BISPHOSPHONIC ACIDS
    5.
    发明申请
    PROCESS FOR MANUFACTURING BISPHOSPHONIC ACIDS 审中-公开
    制备双磷酸的方法

    公开(公告)号：US20090137808A1

    公开(公告)日：2009-05-28

    申请号：US12282725

    申请日：2007-03-16

    申请人： Edward G. Samsel ,  Tse-Chong Wu

    发明人： Edward G. Samsel ,  Tse-Chong Wu

    IPC分类号： C07D221/02 ,  C07D233/54 ,  C07D213/02 ,  C07F9/38

    CPC分类号： C07F9/3873 ,  C07F9/386 ,  C07F9/58 ,  C07F9/6506 ,  C07F9/6561

    摘要： A manufacturing process for the preparation of bisphosphonic acids and in particular zoledronic acid is provided wherein diglyme, monoglyme, or a mixture thereof, is utilized to produce a homogenous, water soluble, solid reaction mass that upon cooling, dissolving in water and stripping results in a high purity product and comparatively good yield. wherein Ri is selected from the group consisting of

    摘要翻译： 提供了制备二膦酸，特别是唑来膦酸的制备方法，其中二甘醇二甲醚，单甘醇二甲醚或其混合物用于产生均匀的水溶性固体反应物质，其在冷却时溶解在水中并且汽提得到 高纯度的产品和较好的产量。 其中R 1选自由以下组成的组

    Process for production of fluoroalkoxy-substituted benzamides and their intermediates
    6.
    发明授权
    Process for production of fluoroalkoxy-substituted benzamides and their intermediates 失效
    制备氟烷氧基取代苯甲酰胺及其中间体的方法

    公开(公告)号：US06822114B1

    公开(公告)日：2004-11-23

    申请号：US10266959

    申请日：2002-10-08

    申请人： Eric L. Williams ,  Tse-Chong Wu

    发明人： Eric L. Williams ,  Tse-Chong Wu

    IPC分类号： C07L6500

    CPC分类号： C07C51/09 ,  C07C43/225 ,  C07C43/23 ,  C07C51/60 ,  C07C2601/02 ,  C07D213/61 ,  C07C65/26

    摘要： Roflumilast and new key intermediates therefor are prepared by processes involving use of carbonylation technology. Good overall yields can be achieved using available starting materials. The starting material for the process can be catechol, an o-R1-phenol, an o-R1-p-X-phenol, or a 1-X-3-R1-4-R2-benzene, where R1, is a C1-6 alkoxy, C3-7 cycloalkoxy, C3-7 cycloalkylmethoxy, or benzyloxy group, or a C1-4 alkoxy group which is completely or partially substituted by fluorine; R2 is a C1-4 alkoxy group which is completely or partially substituted by fluorine; and X is Cl, Br, or I.

    摘要翻译： 罗氟司特及其新型关键中间体是通过涉及使用羰基化技术的方法制备的。 可以使用可用的原料实现良好的总产率。 该方法的起始原料可以是邻苯二酚，o-R1-苯酚，o-R1-pX-苯酚或1-X-3-R1-4-R2-苯，其中R1为C1-6 烷氧基，C 3-7环烷氧基，C 3-7环烷基甲氧基或苄氧基，或被氟完全或部分取代的C 1-4烷氧基; R2是被氟完全或部分取代的C 1-4烷氧基; X为Cl，Br或I.

    Process for preparing olefins
    7.
    发明授权
    Process for preparing olefins 失效
    制备烯烃的方法

    公开(公告)号：US5536870A

    公开(公告)日：1996-07-16

    申请号：US390466

    申请日：1995-02-17

    申请人： Tse-Chong Wu

    发明人： Tse-Chong Wu

    IPC分类号： C07D215/00 ,  B01J31/24 ,  C07B37/04 ,  C07B61/00 ,  C07C2/86 ,  C07C15/52 ,  C07C17/266 ,  C07C25/24 ,  C07C41/30 ,  C07C43/215 ,  C07C45/68 ,  C07C49/796 ,  C07C51/14 ,  C07C67/38 ,  C07C69/612 ,  C07C69/65 ,  C07C69/734 ,  C07C69/738 ,  C07D213/79 ,  C07C69/76 ,  C07C5/09 ,  C07C11/00 ,  C07C19/08

    CPC分类号： C07C51/14 ,  C07B37/04 ,  C07C17/266 ,  C07C2/861 ,  C07C41/30 ,  C07C45/68

    摘要： A process for preparing olefin compounds of the formula ##STR1## where A is aryl, substituted aryl, heteroaryl, substituted heteroaryl, benzyl, substituted benzyl, vinyl or substituted vinyl and R.sub.2, R.sub.3 and R.sub.4 are hydrogen, alkyl, cycloalkyl, alkyl-substituted cycloalkyl, aryl, substituted aryl, alkoxy, alkythio, heteroaryl, substituted heteroaryl, alkanoyl, aroyl, substituted aroyl, heteroarylcarbonyl, substituted heteroarylcarbonyl, trifluoromethyl or halo, which comprises reacting an organic halide of the formula A-X where X is chloro, bromo or iodo with a vinyl or substituted vinyl compound of the formula ##STR2## where R.sub.2, R.sub.3 and R.sub.4 are as previously defined, in the presence of a catalytically effective amount of palladium or the salts of palladium, where palladium has a valence of 1 or 2 and a cyclic ligand of the formula ##STR3## where R' is the same or different than R" and is hydrogen, alkyl or aryl either substituted or unsubstituted and Ar is phenyl, naphthyl, substituted phenyl or substituted naphthyl, substituted phenyl or substituted naphthyl and n is an integer from 3 to 6, to form an activated reaction mixture. Carboxylic acids can be prepared by carbonylation of such olefins.

    摘要翻译： 其中A是芳基，取代的芳基，杂芳基，取代的杂芳基，苄基，取代的苄基，乙烯基或取代的乙烯基，R2，R3和R4是氢，烷基，环烷基，烷基 - 取代的芳基，烷氧基，链烷基，杂芳基，取代的杂芳基，烷酰基，芳酰基，取代的芳酰基，杂芳基羰基，取代的杂芳基羰基，三氟甲基或卤素，其包括使式AX的有机卤化物，其中X是氯，溴或 在钯催化有效量的钯或钯盐存在下，其中R 2，R 3和R 4如前所定义，其中乙烯基或取代的乙烯基化合物具有式“IMAGE”，其中钯的化合价为1或2 和式“IMAGE”的环状配体，其中R'与R“相同或不同，为氢，烷基或芳基取代或未取代，Ar为苯基，萘基，取代的 烯基或取代的萘基，取代的苯基或取代的萘基，n是3至6的整数，以形成活化的反应混合物。 羧酸可以通过这样的烯烃的羰基化制备。

    Mixed ligand catalyst for preparing aryl-substituted aliphatic carboxylic esters
    8.
    发明授权
    Mixed ligand catalyst for preparing aryl-substituted aliphatic carboxylic esters 失效
    用于制备芳基取代的脂族羧酸酯的混合配体催化剂

    公开(公告)号：US5482596A

    公开(公告)日：1996-01-09

    申请号：US186933

    申请日：1994-01-27

    申请人： Tse-Chong Wu

    发明人： Tse-Chong Wu

    IPC分类号： B01J31/22 ,  B01J31/24 ,  C07C51/14 ,  C07C57/30 ,  C07C57/40 ,  C07C67/38 ,  C07C69/612 ,  C07C69/616 ,  C07C51/10

    CPC分类号： C07C51/14 ,  C07C67/38

    摘要： A new process for preparing aryl substituted aliphatic carboxylic acids and their esters is provided. A 1-aryl substituted olefinic compound is reacted with carbon monoxide in the presence of water (in aqueous conditions) or an alcohol (in anhydrous conditions) at a temperature between about 25.degree. C. and about 200.degree. C. An excess of several moles of water or of anhydrous alcohol is preferred. An acid such as hydrochloric acid may also be added. As catalyst, a mixture of a palladium compound and optionally a copper compound with a ligand mixture comprising a compound of the formula (R').sub.3 ZY and a compound of the formula (R").sub.3 Z where each R' and R" are the same or different and is alkyl, aryl or substituted aryl, and Z is any atom that has a Pauling electronegativity of between 1.9 and 2.5 and Y is a member of Group VIA of the Periodic Table of Elements.

    摘要翻译： 提供了制备芳基取代的脂族羧酸及其酯的新方法。 在约25℃至约200℃的温度下，1-芳基取代的烯属化合物在水（在水性条件下）或醇（无水条件）存在下与一氧化碳反应。过量的几摩尔 的水或无水乙醇是优选的。 还可以加入酸如盐酸。 作为催化剂，钯化合物和任选的铜化合物与包含式（R'）3 ZY的化合物和式（R“）3 Z的化合物的配体混合物的混合物，其中每个R'和R”为 相同或不同的是烷基，芳基或取代的芳基，Z是具有1.9至2.5之间的保宁电负性并且Y是元素周期表的VIA族成员的任何原子。

    Catalytic carboxylation process for preparing aryl-substituted aliphatic carboxylic esters
    10.
    发明授权
    Catalytic carboxylation process for preparing aryl-substituted aliphatic carboxylic esters 失效
    用于制备芳基取代的脂肪族羧酸酯的催化羧化方法

    公开(公告)号：US5322959A

    公开(公告)日：1994-06-21

    申请号：US62907

    申请日：1993-05-11

    申请人： Tse-Chong Wu

    发明人： Tse-Chong Wu

    IPC分类号： C07C51/10 ,  C07C67/36 ,  C07C69/76

    CPC分类号： C07C51/10 ,  C07C67/36

    摘要： A new process for preparing aryl substituted aliphatic carboxylic acid esters is provided. A 1-aryl substituted aliphatic halo compound is reacted with carbon monoxide in the presence of an alcohol in anhydrous conditions at a temperature between about 25.degree. C. and about 200.degree. C. An excess of several moles of anhydrous alcohol is preferred. An acid such as hydrochloric acid may also be added. As catalyst, a mixture of palladium or a palladium compound and a copper compound with at least one acid-stable ligand are present.

    摘要翻译： 提供了制备芳基取代的脂族羧酸酯的新方法。 在醇的存在下，在无水条件下，在约25℃至约200℃的温度下，使1-芳基取代的脂族卤代化合物与一氧化碳反应。优选过量的几摩尔无水乙醇。 还可以加入酸如盐酸。 作为催化剂，存在钯或钯化合物与至少一种酸稳定配体的铜化合物的混合物。