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1. 发明授权

US4780561A Preparation process of .alpha.-L-aspartyl-L-phenylalanine methyl ester or hydrochloride thereof 失效
标题翻译： α-L-天冬氨酰-L-苯丙氨酸甲酯或其盐酸盐的制备方法
公开(公告)号：US4780561A
公开(公告)日：1988-10-25
申请号：US131268
申请日：1987-12-09
申请人： Ryuichi Mita , Takeshi Oura , Toshio Katoh , Chojiro Higuchi , Akihiro Yamaguchi
发明人： Ryuichi Mita , Takeshi Oura , Toshio Katoh , Chojiro Higuchi , Akihiro Yamaguchi
IPC分类号： C07K5/06 , C07K5/075 , C07C103/52 , C07C102/00
CPC分类号： C07K5/0613 , Y10S530/801
摘要： Disclosed herein is a process for preparing .alpha.-L-aspartyl-L-phenylalanine methyl ester or its hydrochloride from 5-benzyl-3,6-dioxo-2-piperazine acetic acid or its methyl ester, prepared without using L-penylalanine methyl ester which involves problems in its stability, as a raw material. Specifically, the process comprises: bringing 5-benzyl-3,6-dioxo-2-piperazine acetic acid in the presence of methanol or 5-benzyl-3,6-dioxo-2-piperazine acetic acid methyl ester in the presence or absence of methanol into contact with hydrochloric acid; isolating the thereby deposited .alpha.-L-aspartyl-L-phenylalanine methyl ester hydrochloride; and neutralizing said hydrochloride with an alkali as required. Preparation processes of 5-benzyl-3,6-dioxo-2-piperazine acetic acid or its methyl ester are also disclosed.
摘要翻译：本文公开了一种从不使用L-青霉素甲酯制备的5-苄基-3,6-二氧代-2-哌嗪乙酸或其甲酯制备α-L-天冬氨酰基-L-苯丙氨酸甲酯或其盐酸盐的方法这涉及到其稳定性问题，作为原料。具体地说，该方法包括：在甲醇或5-苄基-3,6-二氧代-2-哌嗪乙酸甲酯的存在下，在存在或不存在下，使5-苄基-3,6-二氧代-2-哌嗪乙酸的甲醇与盐酸接触; 分离由此沉积的α-L-天冬氨酰-L-苯丙氨酸甲酯盐酸盐; 并根据需要用碱中和所述盐酸盐。还公开了5-苄基-3,6-二氧代-2-哌嗪乙酸或其甲酯的制备方法。

2. 发明授权

US4897506A Isolation of alpha-l-aspartyl-l-phenylalanine methyl ester from aqueous medium 失效
标题翻译：从水介质中分离α-1-天冬氨酰-1-苯丙氨酸甲酯
公开(公告)号：US4897506A
公开(公告)日：1990-01-30
申请号：US256838
申请日：1988-10-12
申请人： Ryuichi Mita , Takeshi Oura , Toshio Katoh , Chojiro Higuchi , Akihiro Yamaguchi , Masanobu Ajioka
发明人： Ryuichi Mita , Takeshi Oura , Toshio Katoh , Chojiro Higuchi , Akihiro Yamaguchi , Masanobu Ajioka
IPC分类号： C07K5/072 , C07K5/075
CPC分类号： C07K5/0613
摘要： A method for preparing .alpha.-L-aspartyl-L-phenylalanine methyl ester having improved solubilization by the isolation thereof from an aqueous medium containing at least one additive selected from the group consisting of sodium alginate, sodium salt of carboxymethylcellulose, sodium starch glycolate and sodium polyacrylate.

3. 发明授权

US4801732A Preparation process of .alpha.-L-aspartyl-L-phenylalanine methyl ester 失效
标题翻译： α-L-天冬氨酰-L-苯丙氨酸甲酯的制备方法
公开(公告)号：US4801732A
公开(公告)日：1989-01-31
申请号：US171134
申请日：1988-03-22
申请人： Ryuichi Mita , Takeshi Oura , Chojiro Higuchi , Toshio Katoh , Akihiro Yamaguchi
发明人： Ryuichi Mita , Takeshi Oura , Chojiro Higuchi , Toshio Katoh , Akihiro Yamaguchi
IPC分类号： C07K5/06 , C07K5/075 , C07C101/32 , A23L1/236
CPC分类号： C07K5/0613
摘要： This invention relates to an improved process for preparing .alpha.-L-aspartyl-L-phenylalanine methyl ester. More specifically, it relates to a process for preparing .alpha.-L-aspartyl-L-phenylalanine methyl ester which comprises treating, as a raw material, N-formyl-.alpha.-L-aspartyl-L-phenylalanine in methanol in the presence of an acid to form .alpha.-L-aspartyl-L-phenylalanine dimethyl ester, hydrolyzing the .alpha.-L-aspartyl-L-phenylalanine dimethyl ester by bringing it into contact with hydrochloric acid in the presence of methanol as desired, separating the thereby-precipitated .alpha.-L-aspartyl-L-phenylalanine methyl ester hydrochloride and neutralizing the hydrochloride. Further, this invention also provides a process for preparing .alpha.-L-aspartyl-L-phenylalanine methyl ester capable of using, as a raw material, N-formyl-.alpha.-L-aspartyl-L-phenylalanine which contains N-formyl-.beta.-L-aspartyl-L-phenylalanine in an amount of 30% by weight or less.
摘要翻译：本发明涉及一种制备α-L-天冬氨酰基-L-苯丙氨酸甲酯的改进方法。更具体地说，本发明涉及一种制备α-L-天冬氨酰基-L-苯丙氨酸甲酯的方法，该方法包括在甲醇中存在下，以N-甲酰基-α-天冬氨酰基-L-苯丙氨酸为原料酸形成α-L-天冬氨酰基-L-苯丙氨酸二甲酯，通过使α-L-天冬氨酰-L-苯丙氨酸二甲酯在需要的甲醇存在下与盐酸接触，分离由此沉淀的α -L-天冬氨酰基-L-苯丙氨酸甲酯盐酸盐并中和盐酸盐。此外，本发明还提供一种制备能够以N-甲酰基-β-L-天冬氨酰基-L-苯丙氨酸为原料的α--L-天冬氨酰基-L-苯丙氨酸甲酯的制备方法，该方法含有N-甲酰基-β -L-天冬氨酰基-L-苯丙氨酸，其量为30重量％以下。

4. 发明授权

US4745210A Preparation process of N-formyl-.alpha.-aspartyl phenylalanine 失效
标题翻译： N-甲酰基-α-天冬氨酰苯丙氨酸的制备方法
公开(公告)号：US4745210A
公开(公告)日：1988-05-17
申请号：US804479
申请日：1985-12-04
申请人： Ryuichi Mita , Toshio Katoh , Chojiro Higuchi , Takeshi Oura , Akihiro Yamaguchi
发明人： Ryuichi Mita , Toshio Katoh , Chojiro Higuchi , Takeshi Oura , Akihiro Yamaguchi
IPC分类号： C07K1/02 , C07K5/06 , C07K5/075 , C07C103/52 , C07C102/00
CPC分类号： C07K5/0613
摘要： This invention relates to an improved process for preparing N-formyl-.alpha.- aspartyl phenylalanine. More specifically, it relates to a process for preparing N-formyl-.alpha.-aspartyl phenylalanine by condensating N-formyl aspartic acid anhydride and phenylalanine which comprises effecting the condensation reaction in a water medium while maintaining the pH during the reaction in the range of 7-12 and at a reaction temperature of 50.degree. C. or below.
摘要翻译：本发明涉及一种制备N-甲酰基-α-天冬氨酰苯丙氨酸的改进方法。更具体地，本发明涉及通过冷凝N-甲酰天冬氨酸酐和苯丙氨酸制备N-甲酰基-α-天冬氨酰苯基丙氨酸的方法，其包括在水介质中进行缩合反应，同时将反应期间的pH保持在7 -12，反应温度为50℃以下。

5. 发明授权

US4962222A Preparation process of .alpha.-l-aspartyl-l-phenylalanine methyl ester having low hygroscopicity 失效
标题翻译：具有低吸湿性的α-1-天冬氨酰基-1-苯丙氨酸甲酯的制备方法
公开(公告)号：US4962222A
公开(公告)日：1990-10-09
申请号：US300724
申请日：1989-01-25
申请人： Ryuichi Mita , Toshio Katoh , Chojiro Higuchi , Takeshi Oura , Akihiro Yamaguchi
发明人： Ryuichi Mita , Toshio Katoh , Chojiro Higuchi , Takeshi Oura , Akihiro Yamaguchi
IPC分类号： C07K1/14 , C07K5/06 , C07K5/072 , C07K5/075
CPC分类号： C07K5/0613
摘要： .alpha.-L-Aspartyl-L-phenylalanine methyl ester having low hygroscopicity is prepared by bringing a cake of .alpha.-L-aspartyl-L-phenylalanine methyl ester, which cake has been obtained by solid-liquid separation through a desired preparation process of .alpha.-L-aspartyl-L-phenylalanine methyl ester, into contact with an organic solvent of uniform phase so as to treat the cake with the organic solvent, subjecting the resulting mixture of the cake and organic solvent to solid-liquid separation to obtain a cake, and then drying the last-mentioned cake at a temperature not higher than 60.degree. C. The organic solvent is dry or contains water in an amount up to 30 wt.%.

6. 发明授权

US4918216A Preparation process of .alpha.-l-aspartyl-l-phenyl-alanine methyl ester or hydrohalide thereof 失效
标题翻译： α-1-天冬氨酰基-1-苯基 - 丙氨酸甲酯或其氢卤化物的制备方法
公开(公告)号：US4918216A
公开(公告)日：1990-04-17
申请号：US357618
申请日：1989-05-25
申请人： Ryuichi Mita , Toshio Katoh , Chojiro Higuchi , Takeshi Oura , Akihiro Yamaguchi
发明人： Ryuichi Mita , Toshio Katoh , Chojiro Higuchi , Takeshi Oura , Akihiro Yamaguchi
IPC分类号： A23L27/30 , C07K1/02 , C07K5/06 , C07K5/075
CPC分类号： C07K5/0613
摘要： .alpha.-L-aspartyl-L-phenylalanine methyl ester or the hydrohalide thereof is prepared by esterifying .alpha.-L-aspartyl-L-phenylalanine or .alpha.-L-aspartyl-L-phenylalanine which has been formed in situ by treating an N-protected-.alpha.-L-aspartyl-L-phenylalanine in an aqueous solution of sulfuric acid or a methanol-containing aqueous solution of sulfuric acid in the presence of an alkali metal halide or alkaline earth metal halide in a medium composed of sulfuric acid, water and methanol, thereby to allow the resulting .alpha.-L-aspartyl-L-phenyl-alanine methyl ester to precipitate as its corresponding hydrohalide, and then isolating the hydrohalide; and when the preparation of the methyl ester is desired, neutralizing the hydrohalide.
摘要翻译： α-L-天冬氨酰基-L-苯丙氨酸甲酯或其氢卤化物通过酯化通过将N-保护的N-保护基团经过N-保护基团处理而形成的α-L-天冬氨酰基-L-苯丙氨酸或α-L-天冬氨酰基-L-苯丙氨酸 α-L-天冬氨酰基-L-苯丙氨酸在硫酸水溶液或含甲醇的硫酸水溶液中，在碱金属卤化物或碱土金属卤化物存在下，在由硫酸，水和从而使所得的α-L-天冬氨酰-L-苯基 - 丙氨酸甲酯作为其对应的氢卤酸盐沉淀，然后分离氢卤化物; 并且当需要制备甲酯时，中和氢卤化物。

7. 发明授权

US4778916A Preparation process of .alpha.-L-aspartyl-L-phenylalanine methyl ester or hydrochloride thereof 失效
标题翻译： α-L-天冬氨酰-L-苯丙氨酸甲酯或其盐酸盐的制备方法
公开(公告)号：US4778916A
公开(公告)日：1988-10-18
申请号：US122583
申请日：1987-11-17
申请人： Ryuichi Mita , Toshio Katoh , Chojiro Higuchi , Takeshi Oura , Akihiro Yamaguchi
发明人： Ryuichi Mita , Toshio Katoh , Chojiro Higuchi , Takeshi Oura , Akihiro Yamaguchi
IPC分类号： C07K5/06 , C07K5/075 , C07C103/52 , C07C102/00
CPC分类号： C07K5/0613 , Y10S530/801
摘要： The present invention relates to a process for preparing .alpha.-L-aspartyl-L-phenylalanine methyl ester or its hydrochloride. .alpha.-L-aspartyl-L-phenylalanine methyl ester or its hydrochloride is prepared by a process comprising: condensating N-formyl-L-aspartic acid anhydride and L-phenylalanine in water or in water containing methanol at a pH in the range of 7-12 to form N-formyl-.alpha.-L-aspartyl-L-phenylalanine; acidifying the reaction mixture successively with hydrochloric acid in the presence of methanol without isolating the N-formyl-.alpha.-L-aspartyl-L-phenylalanine so as to bring it into contact with hydrochloric acid in the presence of methanol for reaction and thereby to deposit .alpha.-L-aspartyl-L-phenylalanine methyl ester hydrochloride; separating the .alpha.-L-aspartyl-L-phenylalanine methyl ester hydrochloride; and neutralizing said hydrochloride as required.
摘要翻译：本发明涉及一种制备α-L-天冬氨酰基-L-苯丙氨酸甲酯或其盐酸盐的方法。 α-L-天冬氨酰基-L-苯丙氨酸甲酯或其盐酸盐的制备方法包括：将N-甲酰基-L-天冬氨酸酐和L-苯丙氨酸在水中或含有甲醇的水中在pH为7的范围内缩合 -12以形成N-甲酰基-α-L-天冬氨酰基-L-苯丙氨酸; 在甲醇存在下，依次用盐酸酸化反应混合物，而不分离N-甲酰基-α-天冬氨酰基-L-苯丙氨酸，使其在甲醇存在下与盐酸接触反应，从而沉积 α-L-天冬氨酰-L-苯丙氨酸甲酯盐酸盐; 分离α-L-天冬氨酰-L-苯丙氨酸甲酯盐酸盐; 并根据需要中和所述盐酸盐。

8. 发明授权

US5206413A Method for preparing .alpha.-L-aspartyl-L-phenylalanine methyl ester 失效
标题翻译：制备（ALPHA）-L-阿糖基-L-苯甲酰胺甲酯的方法
公开(公告)号：US5206413A
公开(公告)日：1993-04-27
申请号：US537451
申请日：1990-06-14
申请人： Masanobu Ajioka , Takeshi Oura , Chojiro Higuchi , Toshio Katoh , Akihiro Yamaguchi
发明人： Masanobu Ajioka , Takeshi Oura , Chojiro Higuchi , Toshio Katoh , Akihiro Yamaguchi
IPC分类号： C07K1/02 , A23L27/30 , C07K1/14 , C07K5/06 , C07K5/075
CPC分类号： C07K5/0613
摘要： A method for preparing .alpha.-L-aspartyl-L-phenylalanine methyl ester (.alpha.-APM), substantially free from acid ion contamination, is disclosed which comprises the steps of contacting a solution of a mineral acid salt or an organic sulfonic acid salt of .alpha.-APM in an aqueous solvent with an anion exchange resin in free base form, separating the resin from the thus-produced solution of .alpha.-APM; and isolating the .alpha.-APM therefrom, preferably with regeneration and recycling the resin.

9. 发明授权

US5113009A Preparation and isolation of mineral acid salt of an amino acid methyl ester 失效
标题翻译：氨基酸甲酯的矿酸盐的制备和分离
公开(公告)号：US5113009A
公开(公告)日：1992-05-12
申请号：US457076
申请日：1989-12-26
申请人： Masanobu Ajioka , Chojiro Higuchi , Takeshi Oura , Toshio Katoh , Akihiro Yamaguchi
发明人： Masanobu Ajioka , Chojiro Higuchi , Takeshi Oura , Toshio Katoh , Akihiro Yamaguchi
IPC分类号： C07C227/18 , C07C227/40
CPC分类号： C07C227/40 , C07C227/18
摘要： A cyclical process for producing and isolating a mineral acid salt of an amino acid methyl ester in high purity and yield from the reaction solution produced by esterifying an amino acid with methanol in methanol in the presence of a mineral acid, by cooling the resulting reaction solution to precipitate crystals of the mineral acid salt; filtering the crystals;drying the isolated wet crystals or washing with another organic solvent; and recycling the filtrate for reuse in the esterification reaction.

10. 发明授权

US5302743A Preparation of N-protected .alpha.-L-aspartyl-L-phenylalanine methyl ester 失效
标题翻译： N-保护的α-L-天冬氨酰基-L-苯丙氨酸甲酯的制备
公开(公告)号：US5302743A
公开(公告)日：1994-04-12
申请号：US823538
申请日：1992-01-21
申请人： Toshio Katoh , Chojiro Higuchi , Takeshi Oura , Masanobu Ajioka , Akihiro Yamaguchi
发明人： Toshio Katoh , Chojiro Higuchi , Takeshi Oura , Masanobu Ajioka , Akihiro Yamaguchi
IPC分类号： C07K5/075 , C07C229/00
CPC分类号： C07K5/0613 , Y02P20/55
摘要： Disclosed is an improved process for the preparation of an N-protected .alpha.-L-aspartyl-L-phenylalanine methyl ester from an N-protected L-aspartic anhydride and L-phenylalanine methyl ester, the improvement which comprises employing the L-phenylalanine methyl ester in the form of a mineral acid salt thereof and conducting the reaction either (a) in an organic solvent and in the presence of a salt of an organic carboxylic acid, or (b) in an organic solvent comprising an organic carboxylic acid and in the presence of at least one member of the group consisting of an alkali metal or an alkaline earth metal inorganic base, an ammonium alkali metal or alkaline earth metal salt of an organic carboxylic acid and ammonium carbonate. The starting N-protected aspartic anhydride, e.g., N-benzyloxycarbonyl-L-aspartic anhydride, can be produced by the reaction of N-protected aspartic acid with phosgene. When the N-protecting group sibenzyloxycarbonyl and the solvent is acetic acid, the desired product can be isolated from the reaction mixture in crystalline form in high purity by adding water thereto.
摘要翻译：公开了一种由N-保护的L-天冬氨酸酐和L-苯丙氨酸甲酯制备N-保护的α-L-天冬氨酰-L-苯丙氨酸甲酯的改进方法，其改进包括使用L-苯丙氨酸甲酯酯，其为无机酸盐，并且在有机溶剂中和有机羧酸的盐存在下进行反应，或（b）在包含有机羧酸的有机溶剂中和存在由碱金属或碱土金属无机碱组成的组中的至少一种，有机羧酸的铵碱金属或碱土金属盐和碳酸铵。起始的N-保护的天冬氨酸酐，例如N-苄氧基羰基-L-天冬氨酸酐可以通过N-保护的天冬氨酸与光气的反应来制备。当N-保护基团苄氧基羰基和溶剂为乙酸时，可以通过向其中加入水从所述反应混合物中以高纯度从结晶形式中分离所需产物。

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