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11. 发明授权

US5225587A Method of producing .alpha.-L-aspartyl-L-phenylalanine methyl ester hydrochloride 失效
标题翻译：生产α-L-天冬氨酰-L-苯丙氨酸甲酯盐酸盐的方法
公开(公告)号：US5225587A
公开(公告)日：1993-07-06
申请号：US864133
申请日：1992-04-06
申请人： Katsumi Sugiyama , Kiyo Adachi , Toshihide Yukawa
发明人： Katsumi Sugiyama , Kiyo Adachi , Toshihide Yukawa
IPC分类号： C07K5/072 , C07K5/075
CPC分类号： C07K5/0613
摘要： A method of purifying .alpha.-L-aspartyl-L-phenylalanine methyl ester as a hydrochloride salt thereof which comprises:i) contacting a mixture of .alpha.-L-aspartyl-L-phenylanaline methyl ester and .beta.-L-aspartyl-L-phenylalanine methyl ester with an aqueous medium containing (a) hydrogen chloride in an amount not more than ca. 2 mol., per liter of said aqueous medium, but not less than 1 mol., per mole of said of said mixture of .alpha.-L-aspartyl-L-phenylalanine methyl ester and .beta.-L-aspartyl-L-phenylalanine methyl ester, and (b) an inorganic chloride selected from the group consisting of NaCl, KCl, NH.sub.4 Cl, CaCl.sub.2, and ZnCl.sub.2 in an amount of at least ca. 50 g., per liter of said aqueous medium, to form crystals of .alpha.-L-aspartyl-L-phenylalanine methyl ester hydrochloride, andii) recovering the .alpha.-L-aspartyl-L-phenylalanine methyl ester hydrochloride crystals therefrom.
摘要翻译：纯化α-L-天冬氨酰基-L-苯丙氨酸甲酯盐酸盐的方法，其包括：i）使α-L-天冬氨酰基-L-苯亚胺甲酯与β-L-天冬氨酰基-L-苯丙氨酸的混合物甲酯与含有（a）氯化氢的含水介质的量不大于约每摩尔所述所述α-L-天冬氨酰基-L-苯丙氨酸甲酯和β-L-天冬氨酰-L-苯丙氨酸甲酯的混合物每升所述水性介质2摩尔，但不小于1摩尔，和（b）选自NaCl，KCl，NH 4 Cl，CaCl 2和ZnCl 2的无机氯化物，其量至少约为。 50升，每升所述水性介质中，形成α-L-天冬氨酰基-L-苯丙氨酸甲酯盐酸盐的晶体，和ii）从其中回收α-L-天冬氨酰基-L-苯丙氨酸甲酯盐酸盐晶体。

12. 发明授权

US4822907A Method for recovering .alpha.-L-aspartyl-L-phenylalanine methyl ester 失效
标题翻译： α-L-天冬氨酰-L-苯丙氨酸甲酯的回收方法
公开(公告)号：US4822907A
公开(公告)日：1989-04-18
申请号：US56907
申请日：1987-06-03
申请人： Katsumi Sugiyama , Takashi Yamashita , Toshihide Yukawa
发明人： Katsumi Sugiyama , Takashi Yamashita , Toshihide Yukawa
IPC分类号： C07K1/14 , C07K1/26 , C07K5/072 , C07K5/075 , C07C103/52
CPC分类号： C07K5/0613
摘要： A process for recovering .alpha.-L-aspartyl-L-phenylalanine methyl ester from a solution containing various methyl ester or demethylated derivatives of .alpha.-L-aspartyl-L-phenylalanine methyl ester and chloride ions is disclosed. This process uses a reverse osmosis membrane having a specific chloride inhibition rate to desalt and concentrate a solution containing a specified ratio of .delta.-L-aspartyl-L-phenylalanine methyl ester to its derivatives until a specific weight ratio of organic chloride ion to the sum of .alpha.-L-aspartyl-L-phenylalanine methyl ester and its derivatives is obtained. This desalted and concentrated solution is then contacted with an aqueous solvent containing methanol and hydrochloride acid to recover high yields of .alpha.-L-aspartyl-L-phenylalanine methyl ester hydrochloride.
摘要翻译：公开了从含有α-L-天冬氨酰-L-苯丙氨酸甲酯和氯离子的各种甲酯或去甲基化衍生物的溶液中回收α-L-天冬氨酰基-L-苯丙氨酸甲酯的方法。该方法使用具有特定氯化物抑制速率的反渗透膜脱盐，并将含有特定比例的δ-L-天冬氨酰-L-苯丙氨酸甲酯的溶液浓缩至其衍生物，直到有机氯离子与总和的比重的α-L-天冬氨酰基-L-苯丙氨酸甲酯及其衍生物。然后将该脱盐浓缩溶液与含有甲醇和盐酸的含水溶剂接触，以回收高产率的α-L-天冬氨酰基-L-苯丙氨酸甲酯盐酸盐。

13. 发明授权

US4820861A Process for the production of N-formyl-alpha-L-aspartyl-L-phenylalanine methyl ester 失效
标题翻译：制备N-甲酰基-α-L-天冬氨酰基-L-苯丙氨酸甲酯的方法
公开(公告)号：US4820861A
公开(公告)日：1989-04-11
申请号：US931123
申请日：1986-11-17
申请人： Toshihide Yukawa , Haruo Kawasaki , Masao Nakamura , Takashi Yamashita , Toshiaki Tsuji
发明人： Toshihide Yukawa , Haruo Kawasaki , Masao Nakamura , Takashi Yamashita , Toshiaki Tsuji
IPC分类号： C07K1/06 , B01J31/04 , C07B61/00 , C07K5/06 , C07K5/075 , C07C101/02
CPC分类号： C07K5/0613
摘要： N-formyl-.alpha.-L-aspartyl-L-phenylalanine methyl ester is obtained by reacting L-phenylalanine methyl ester with N-formyl-L-aspartic acid anhydride in a reaction solvent containing acetic acid or acetic acid and formic acid in a complete mixing type continuous reaction mode.
摘要翻译： N-甲酰基-α-天冬氨酰基-L-苯丙氨酸甲酯通过L-苯丙氨酸甲酯与N-甲酰基-L-天冬氨酸酐在含有乙酸或乙酸的反应溶剂和甲酸的完全反应溶液中反应得到混合型连续反应方式。

14. 发明授权

US5451671A Method of purifying 2',3'-dideoxynucleosides 失效
标题翻译： 2'，3'-双脱氧核苷的纯化方法
公开(公告)号：US5451671A
公开(公告)日：1995-09-19
申请号：US76964
申请日：1993-06-16
申请人： Hiroshi Shiragami , Masayuki Arai , Kunisuke Izawa , Yutaka Honda , Yasuhiro Tanaka , Toshihide Yukawa , Satoji Takahashi
发明人： Hiroshi Shiragami , Masayuki Arai , Kunisuke Izawa , Yutaka Honda , Yasuhiro Tanaka , Toshihide Yukawa , Satoji Takahashi
IPC分类号： C07H1/06 , C07H19/04 , C07H19/173
CPC分类号： C07H1/06 , C07H19/04
摘要： A crude 2',3'-dideoxynucleoside compound is purified by extracting with an organic solvent, or crystallizing, the 2',3'-dideoxynucleoside compound from a basic aqueous solution having a pH of not less than 12 containing the same. In another embodiment of purification a basic aqueous solution having a pH of not less than 11 of a crude 2',3'-dideoxynucleoside derivative is brought into contact with a nonpolar porous resin, whereby the derivative is adsorbed on the resin, and then the thus adsorbed derivative is desorbed with an aqueous alcoholic solution.2',3'-Dideoxynucleoside compounds which have utility as anti-AIDS drugs or anti-virus drugs can be isolated and purified in high purity and in high yield from their crude products containing impurities.
摘要翻译：粗制的2'，3'-二脱氧核苷化合物通过用有机溶剂萃取，或从含有其的pH不低于12的碱性水溶液中结晶2'，3'-二脱氧核苷化合物而纯化。在纯化的另一个实施方案中，使粗制的2'，3'-二脱氧核苷衍生物的pH不低于11的碱性水溶液与非极性多孔树脂接触，由此将衍生物吸附在树脂上，然后将因此吸附的衍生物用含水醇溶液解吸。具有作为抗艾滋病药物或抗病毒药物的作用的2'，3'-二脱氧核苷化合物可以从其含有杂质的粗产物中以高纯度和高产率分离和纯化。

15. 发明授权

US4610827A Amino acid complex and a method for optical resolution of a DL-amino acid 失效
标题翻译：氨基酸复合物和DL-氨基酸的光学拆分方法
公开(公告)号：US4610827A
公开(公告)日：1986-09-09
申请号：US629468
申请日：1984-07-10
申请人： Toshihide Yukawa , Toru Ikeda , Shinichi Kishimoto , Katsumi Sugiyama
发明人： Toshihide Yukawa , Toru Ikeda , Shinichi Kishimoto , Katsumi Sugiyama
IPC分类号： C07B57/00 , C07C67/00 , C07C227/34 , C07C229/02 , C07C229/36 , C07C239/00 , C07C271/22 , C07C301/00 , C07C323/58 , C07D209/20 , C07C103/50
CPC分类号： C07C271/22
摘要： A method for optical resolution of a DL-amino acid comprising reacting the DL-amino acid with an optically active N-acyl aspartic acid in a solvent or mixture of solvents, and separating the resulting two diasteromeric salts by way of the difference between their solubilities in the solvent or mixture of solvents. The difference in solubility may be enhanced by cooling, concentration, addition of a solubility-decreasing organic solvent, pH adjustment or salting out.
摘要翻译：一种DL-氨基酸的光学拆分方法，包括将DL-氨基酸与光学活性N-酰基天冬氨酸在溶剂或溶剂混合物中反应，并通过其溶解度之间的差异分离得到的两种非对映异构体盐在溶剂或溶剂混合物中。通过冷却，浓缩，添加溶解度降低的有机溶剂，pH调节或盐析可以提高溶解度的差异。

16. 发明授权

US5958977A Phosphoric acid-amino acid complex salt and additive composition containing the salt and used in feed for ruminant mammals 失效
标题翻译：磷酸 - 氨基酸配盐和含有盐的添加剂组合物，用于反刍哺乳动物饲料
公开(公告)号：US5958977A
公开(公告)日：1999-09-28
申请号：US687428
申请日：1996-08-09
申请人： Toru Ikeda , Toshihide Yukawa
发明人： Toru Ikeda , Toshihide Yukawa
IPC分类号： C07F9/09 , A23K20060101 , A23K1/00 , A23K1/16 , A23K1/18 , C01B25/28 , C07C229/26 , C07C279/14 , C07F20060101 , C07F9/00 , A23K1/175
CPC分类号： C07C279/14 , A23K20/147 , A23K40/35 , A23K50/10 , C07C229/26 , Y10S426/807 , Y10S514/905
摘要： A novel phosphoric acid-amino acid complex salt is provided which manifests insolubility in a neutral or alkaline aqueous solution and solubility in an acidic aqueous solution and has a basic amino acid, an alkaline earth metal, and phosphoric acid as main components thereof. An additive composition containing the complex salt and used in a feed for ruminant mammals excels in protection in the first compartment of the stomach of a ruminant mammal and solubility in the fourth compartment of the stomach. This additive composition improves the nutrition of the feed with respect to such a basic amino acid as lysine, a substance frequently missing in the feed for ruminant mammals.
摘要翻译： PCT No.PCT / JP95 / 02530 Sec。 371日期：1996年8月9日 102（e）日期1996年8月9日PCT提交1995年12月8日PCT公布。第WO96 / 17822号公报日期1996年6月13日提供了一种新的磷酸 - 氨基酸配盐，其在中性或碱性水溶液中表现出不溶性，在酸性水溶液中的溶解度为碱性氨基酸，碱土金属和磷酸为主要其组件。含有复盐并用于反刍动物哺乳动物的饲料中的添加剂组合物在反刍动物哺乳动物的胃的第一隔室中的保护性和在胃的第四隔室中的溶解性优异。这种添加剂组合物相对于诸如赖氨酸这样的碱性氨基酸改善了饲料的营养，赖氨酸是反刍哺乳动物饲料中经常缺失的物质。

17. 发明授权

US5179009A Process for producing L-aspartyl-L-phenylalanine and its diketopiperazine 失效
标题翻译： L-天冬氨酰-L-苯丙氨酸及其二酮哌嗪的制备方法
公开(公告)号：US5179009A
公开(公告)日：1993-01-12
申请号：US707306
申请日：1991-05-29
申请人： Kenzo Yokozeki , Naoki Usui , Toshihide Yukawa , Yoshiteru Hirose , Koji Kubota
发明人： Kenzo Yokozeki , Naoki Usui , Toshihide Yukawa , Yoshiteru Hirose , Koji Kubota
IPC分类号： C07D241/08 , C07K5/072 , C07K5/075 , C12P17/12
CPC分类号： C07D241/08 , C07K5/0613 , C12P17/12 , Y10S435/822
摘要： The present invention is directed to a process for producing L-aspartyl-L-phenylalanine and/or L-aspartyl-L-phenylalanine diketopiperazine comprising contacting and reacting a culture, cell or a cell-treated product of a microorganism capable of hydrolyzing DKP into AP or capable of performing intramolecular condensation of AP into DKP with DKP and/or AP, in an aqueous medium.
摘要翻译：本发明涉及一种L-天冬氨酰基-L-苯丙氨酸和/或L-天冬氨酰基-L-苯丙氨酸二酮哌嗪的制备方法，其包括将能够水解DKP的微生物的培养物，细胞或细胞处理的产物与 AP或能够在水性介质中使用DKP和/或AP在AP中进行DK分子内缩合。

18. 发明授权

US4670568A Process of producing n-formylaspartic anhydride 失效
标题翻译：生产N-甲酰基天冬氨酸酐的方法
公开(公告)号：US4670568A
公开(公告)日：1987-06-02
申请号：US792553
申请日：1985-10-29
申请人： Masao Nakamura , Hideo Takeda , Toshihide Yukawa , Haruo Kawasaki
发明人： Masao Nakamura , Hideo Takeda , Toshihide Yukawa , Haruo Kawasaki
IPC分类号： C07D307/60 , C07D307/66
CPC分类号： C07D307/66
摘要： A process for producing N-formylaspartic anhydride, which comprises, grinding solid aspartic acid into fine particles; and then reacting said finely ground aspartic acid with formic acid and acetic anhydride.
摘要翻译：一种生产N-甲酰天冬氨酸酐的方法，其包括将固体天冬氨酸研磨成细颗粒; 然后使所述精细研磨的天冬氨酸与甲酸和乙酸酐反应。

19. 发明授权

US4666838A Process for the production of L-aspartyl-L-phenylalanine esters 失效
标题翻译： L-天冬氨酰-L-苯丙氨酸酯的制备方法
公开(公告)号：US4666838A
公开(公告)日：1987-05-19
申请号：US707808
申请日：1985-03-04
申请人： Kenzo Yokozeki , Eiji Majima , Yoshiteru Hirose , Takeru Sato , Toshihide Yukawa
发明人： Kenzo Yokozeki , Eiji Majima , Yoshiteru Hirose , Takeru Sato , Toshihide Yukawa
IPC分类号： C07K5/072 , C07K5/075 , C12P21/02 , C12N1/14 , C12N1/18 , C12N1/20
CPC分类号： C07K5/0613 , Y10S435/822 , Y10S435/83 , Y10S435/84 , Y10S435/843 , Y10S435/849 , Y10S435/85 , Y10S435/859 , Y10S435/91 , Y10S435/911 , Y10S435/921 , Y10S435/942
摘要： A process for producing L-aspartyl-L-phenylalanine alkyl or aryl esters wherein L-aspartic acid and L-phenylalanine which is esterified with an alkyl group having at least two carbon atoms, an aryl group or an aralkyl group, are contacted in an aqueous medium with particular microorganisms or enzyme fractions from these microorganisms and the condensed product crystallizes out due to insolubility in the aqueous medium.
摘要翻译：一种L-天冬氨酰基-L-苯丙氨酸烷基或芳基酯的制备方法，其中用具有至少两个碳原子的烷基（芳基或芳烷基）酯化的L-天冬氨酸和L-苯丙氨酸在具有特定微生物的水性介质或来自这些微生物的酶部分，并且冷凝产物由于在水性介质中的不溶性而结晶出来。

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