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    Process for the production of 1,2-dithiolan-3-pentanoic acid (thioctic acid) and 8-hydrocarbylthio-6-oxooctanoic acid
    1.
    发明授权
    Process for the production of 1,2-dithiolan-3-pentanoic acid (thioctic acid) and 8-hydrocarbylthio-6-oxooctanoic acid 失效
    生产1,2-二硫戊环-3-戊酸（硫辛酸）和8-烃基硫代-6-氧代辛酸的方法

    公开(公告)号：US4966732A

    公开(公告)日：1990-10-30

    申请号：US73584

    申请日：1987-07-15

    申请人： Guenes Giray ,  Klaus Huthmacher ,  Axel Kleemann ,  Thomas Lied

    发明人： Guenes Giray ,  Klaus Huthmacher ,  Axel Kleemann ,  Thomas Lied

    IPC分类号： C07C323/52 ,  A61K31/385 ,  A61P1/16 ,  A61P25/00 ,  C07C67/00 ,  C07C313/00 ,  C07C319/06 ,  C07C319/14 ,  C07C319/20 ,  C07C323/22 ,  C07C327/22 ,  C07D339/04

    CPC分类号： C07D339/04 ,  C07C323/00

    摘要： 1,2-Dithiolane-3-pentanoic acid (D,L-thioctic acid) of the formula ##STR1## is prepared by a process comprising (a) reacting a 2-(3-alkylthiopropionyl)-cyclopentanone-1 of the formula ##STR2## where R is a C.sub.1 -C.sub.4 alkyl, phenyl or benzyl in aqueous alkaline solution at a temperature of about 20.degree. C. to about 90.degree. C. to form the corresponding carboxylic acid of formula VI ##STR3## (b) reacting the compound of formula VI with an alkyl mercaptan at a temperature between -20.degree. C. and 0.degree. C. to form the corresponding thioketal of formula VII ##STR4## (c) reacting the compound of formula VII with sodium in liquid ammonia at temperature temperture between -60.degree. C. and -10.degree. C. to form the 6,8-dimercaptooctanic acid of formual VIII ##STR5## (d) reacting the 6,8-dimercaptooctanoic acid of formula VIII in alkaline solution with an iron (III) salt and oxygen to form the 1,2-dithiolane-3-pentanoic acid of formula IX, or in place of steps (a) through (c) reacting an acid of formula XII ##STR6## where R.sub.1 and R.sub.2 are hydrogen, C.sub.1 -C.sub.4 -alkyl, phenyl or benzyl, with the proviso that both R.sub.1 and R.sub.2 cannot be benzyl, with sodium in liquid ammonia at a temperature between -60.degree. C. and -10.degree. C. to form the corresponding 6,8-dimercaptooctanoic acid of formula VIII. The compounds of formulae VI, VII, XII are new.

    Process for the production of 1,2-dithiolan-3-pentanoic acid (thioctic acid) and intermediate compounds therefor
    2.
    发明授权
    Process for the production of 1,2-dithiolan-3-pentanoic acid (thioctic acid) and intermediate compounds therefor 失效
    生产1,2-二硫戊环-3-戊酸（硫辛酸）及其中间体化合物的方法

    公开(公告)号：US4705867A

    公开(公告)日：1987-11-10

    申请号：US848212

    申请日：1986-04-04

    申请人： Guenes Giray ,  Klaus Huthmacher ,  Axel Kleemann ,  Thomas Lied

    发明人： Guenes Giray ,  Klaus Huthmacher ,  Axel Kleemann ,  Thomas Lied

    IPC分类号： C07C323/52 ,  A61K31/385 ,  A61P1/16 ,  A61P25/00 ,  C07C67/00 ,  C07C313/00 ,  C07C319/06 ,  C07C319/14 ,  C07C319/20 ,  C07C323/22 ,  C07C327/22 ,  C07D339/04

    CPC分类号： C07D339/04 ,  C07C323/00

    摘要： 1,2-Dithiolane-3-pentanoic acid (D,L-thioctic acid) of the formula ##STR1## is prepared by a process comprising (a) reacting a 2-(3-alkylthiopropionyl)-cyclopentanone-1 of the formula ##STR2## where R is a C.sub.1 -C.sub.4 alkyl, phenyl or benzyl in aqueous alkaline solution at a temperature of about 20.degree. C. to about 90.degree. C. to form the corresponding carboxylic acid of formula VI ##STR3## (b) reacting the compound of formula VI with an alkyl mercaptan at a temperature between -20.degree. C. and 0.degree. C. to form the corresponding thioketal of formula VII ##STR4## (c) reacting the compound of formula VII with sodium in liquid ammonia at a temperature between -60.degree. C. and -10.degree. C. to form the 6,8-dimercaptooctanoic acid of formula VIII ##STR5## (d) reacting the 6,8-dimercaptooctanoic acid of formula VIII in alkaline solution with an iron (III) salt and oxygen to form the 1,2-dithiolane-3-pentanoic acid of formula IX, or in place of steps (a) through (c) reacting an acid of formula XII ##STR6## where R.sub.1 and R.sub.2 are hydrogen, C.sub.1 -C.sub.4 -alkyl, phenyl or benzyl, with the proviso that both R.sub.1 and R.sub.2 cannot be benzyl, with sodium in liquid ammonia at a temperature between -60.degree. C. and -10.degree. C. to form the corresponding 6,8-dimercaptooctanoic acid of formula VIII. The compounds of formulae VI, VII, XII are new.

    摘要翻译： 式（IX）的1,2-二硫戊环-3-戊酸（D，L-硫辛酸）是通过以下方法制备的，该方法包括：（a）使式（I）的2-（3-烷硫基丙酰基） - 环戊酮-1 V，其中R是在约20℃至约90℃的温度下在碱性水溶液中的C 1 -C 4烷基，苯基或苄基，以形成相应的式VI的羧酸 ）使式Ⅵ化合物与烷基硫醇在-20℃至0℃之间的温度下反应，形成相应的式Ⅶ的缩酮醛Ⅶ（c）使式Ⅶ化合物与液体中的钠反应 在-60℃至-10℃的温度下加入氨以形成式VIII的6,8-二巯基辛酸VIII（d）使式VIII的6,8-二巯基辛酸在碱性溶液中与 铁（III）盐和氧气以形成式IX的1,2-二硫戊环-3-戊酸，或代替步骤（a）至（c）使式XI的酸 其中R 1和R 2是氢，C 1 -C 4 - 烷基，苯基或苄基，条件是R 1和R 2不能是苄基，钠在液氨中在-60℃和-60℃之间， 10℃，形成相应的式VIII的6,8-二巯基辛酸。 式VI，VII，XII的化合物是新的。

    Method of preparing 1,6-di(N.sup.3 -cyano-N.sup.1 -guanidino) hexane
    4.
    发明授权
    Method of preparing 1,6-di(N.sup.3 -cyano-N.sup.1 -guanidino) hexane 失效
    制备1,6-二（N 3 - 氰基-N 1胍基）己烷的方法

    公开(公告)号：US5041655A

    公开(公告)日：1991-08-20

    申请号：US241116

    申请日：1988-09-06

    申请人： Klaus Huthmacher ,  Axel Kleemann ,  Horst Bethge ,  Rolf Braun

    发明人： Klaus Huthmacher ,  Axel Kleemann ,  Horst Bethge ,  Rolf Braun

    IPC分类号： C07C67/00 ,  C07C239/00 ,  C07C277/08 ,  C07C279/28

    CPC分类号： C07C279/28

    摘要： An improved method of preparing 1,6-di(N.sup.3 -cyano-N.sup.1 -guanidino) hexane from alkali dicyanamide and a hexamethylene diammonium salt in alcoholic solution or suspension. The reaction is carried out in the presence of a limited amount of water and of a catalytic amount of a base, preferably a tertiary amine. The pH of the reaction mixture at the start of the reaction is 8 to 10. After the reaction is over, the reaction mixture is compounded with water at a temperature above 80.degree. C. and the coarse product which crystallizes out is separated from the liquid phase.Preferably, sodium dicyanamide and hexamethylene diamine dihydrochloride, preferably formed in situ from aqueous 1,6-diaminohexane and aqueous hydrochloric acid, are reacted at pH 9-9.5 in n-butanol in the presence of 0.1 to 20% by wt. water in relation to the solvent including water.1,6-di(N.sup.3 -cyano-N.sup.1 -guanidino) hexane is obtained in a high yield (85-86%) and with great purity (95-97%) and with a considerably improved space-time yield.

    摘要翻译： 一种在醇溶液或悬浮液中由碱二氰胺和六亚甲基二铵盐制备1,6-二（N 3 - 氰基-N 1胍基）己烷的改进方法。 反应在有限量的水和催化量的碱，优选叔胺的存在下进行。 反应开始时反应混合物的pH值为8〜10。反应结束后，将反应混合物在高于80℃的温度下与水混合，将结晶出来的粗产物与液体分离 相。 优选地，优选在1,6-二氨基己烷水溶液和盐酸水溶液中原位形成的二氰胺钠和六亚甲基二胺盐酸盐在pH为9-9.5的正丁醇中，在0.1-20重量％的存在下反应。 相对于包括水在内的溶剂的水。 以高产率（85-86％）和高纯度（95-97％）获得1,6-二（N 3 - 氰基-N 1胍基）己烷，并具有显着提高的时空产率。

    PROCESS FOR THE PREPARATION OF METHIONINE
    8.
    发明申请
    PROCESS FOR THE PREPARATION OF METHIONINE 有权
    制备甲硫氨酸的方法

    公开(公告)号：US20150051421A1

    公开(公告)日：2015-02-19

    申请号：US14386165

    申请日：2013-02-26

    申请人： Martin Koerfer ,  Hans Joachim Hasselbach ,  Stefan Reichert ,  Harald Jakob ,  Christoph Weckbecker ,  Klaus Huthmacher ,  Horst Krull ,  Bernd Drapal ,  Rainer Peter

    发明人： Martin Koerfer ,  Hans Joachim Hasselbach ,  Stefan Reichert ,  Harald Jakob ,  Christoph Weckbecker ,  Klaus Huthmacher ,  Horst Krull ,  Bernd Drapal ,  Rainer Peter

    IPC分类号： C07C319/12 ,  C07C323/52

    CPC分类号： C07C319/28 ,  C07C319/12 ,  C07C319/20 ,  C07C319/26 ,  C07C323/52 ,  Y02P20/142 ,  C07C323/58

    摘要： The invention relates to a process for the preparation of D,L-methionine, in which carbon dioxide is fed to an aqueous potassium methioninate solution obtained by hydrolysis of 5-(2-methylmercaptoethyl)hydantoin, in order to precipitate out crude methionine, which is separated off and purified, where, for the purposes of purification, an aqueous solution of the separated-off crude methionine is prepared and subjected to a recrystallization, characterized in that the solution from which the recrystallization takes place contains potassium ions and also a crystallization additive, where the crystallization additive is a nonionic or anionic surfactant, or a mixture of different nonionic or anionic surfactants, and that the recrystallization takes place by introducing a 60 to 110° C.-hot methionine solution into a 35 to 80° C.-warm methionine suspension, the temperature of which is lower than that of the introduced solution, the temperature of the methionine suspension being maintained between 35 and 80° C. during the addition.

    摘要翻译： 本发明涉及一种制备D，L-甲硫氨酸的方法，其中将二氧化碳加入到通过5-（2-甲基巯基乙基）乙内酰脲的水解获得的甲硫氨酸钾水溶液中，以沉淀出粗蛋氨酸， 分离纯化，其中，为了纯化的目的，制备分离的粗制甲硫氨酸的水溶液并进行重结晶，其特征在于进行重结晶的溶液含有钾离子并且还具有结晶 添加剂，其中结晶添加剂是非离子或阴离子表面活性剂，或不同的非离子或阴离子表面活性剂的混合物，并且通过将60至110℃的热甲硫氨酸溶液引入35至80℃进行重结晶。 - 温血蛋氨酸悬浮液，其温度低于引入溶液的温度，甲硫氨酸悬浮液的温度维持在 在加入过程中在35和80℃之间。