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1. 发明授权

US5530155A Process for recovering L-phenylalanine 失效
标题翻译：回收L-苯丙氨酸的方法
公开(公告)号：US5530155A
公开(公告)日：1996-06-25
申请号：US409980
申请日：1995-03-24
申请人： Toyoto Hijiya , Chiaki Mochizuki , Tadashi Takemoto , Kazutaka Nagashima
发明人： Toyoto Hijiya , Chiaki Mochizuki , Tadashi Takemoto , Kazutaka Nagashima
IPC分类号： C07C227/42 , C07C227/40 , C07C229/36 , C07K5/075 , C07C229/34
CPC分类号： C07C227/40
摘要： Addition of a reaction mixture obtained by the mineral acid hydrolysis of at least one side flow generated from the production of .alpha.-L-aspartyl-L-phenylalanine methyl ester to a crystallization slurry containing L-phenylalanine while maintaining the pH of the slurry at 3-8 by adding aqueous alkali affords crystallized L-phenylalanine having a low water content in a high yield.
摘要翻译：将由α-L-天冬氨酰基-L-苯丙氨酸甲酯的产生产生的至少一个侧流的无机酸水解获得的反应混合物加入含有L-苯丙氨酸的结晶浆料中，同时将浆料的pH保持在3 -8，通过加入碱水，以高收率提供低含水率的结晶L-苯丙氨酸。

2. 发明申请

US20050014972A1 Novel intermediate for sweetener with high sweetness and process for producing the same 审中-公开
标题翻译：具有高甜度的甜味剂的新型中间体和生产相同的方法
公开(公告)号：US20050014972A1
公开(公告)日：2005-01-20
申请号：US10918344
申请日：2004-08-16
申请人： Shigeru Kawahara , Kenichi Mori , Kazutaka Nagashima , Tadashi Takemoto
发明人： Shigeru Kawahara , Kenichi Mori , Kazutaka Nagashima , Tadashi Takemoto
IPC分类号： C07C45/41 , C07C47/277 , C07C51/367 , C07C303/30 , C07C309/66 , C07K5/072 , C07K5/075 , C07C65/03
CPC分类号： C07C51/367 , C07C45/41 , C07C47/277 , C07C303/30 , C07K5/06113 , C07C59/64 , C07C309/66
摘要： The present invention relates to a 3-substituted-phenyl-3-merthylbutyric acid and 3-substituted-phenyl-3-merthylaldehyde derivatives, which are useful in the production of N-[N-[3-(3-hydroxy-4-methoxyphenyl)-3-methylbutyl]-L-α-aspartyl]-L-phenylalanine 1-methyl ester, which is a sweetener with high sweetening potency.
摘要翻译：本发明涉及3-取代的苯基-3-三甲基丁酸和3-取代的苯基-3-甲基乙醛衍生物，其可用于制备N- [N- [3-（3-羟基-4- 甲氧基苯基）-3-甲基丁基] -L-α-天冬氨酰基] -L-苯丙氨酸1-甲基酯，其是具有高甜味效力的甜味剂。

3. 发明授权

US06822111B2 Process for production of aspartyl dipeptide ester derivatives 失效
标题翻译：天冬氨酰二肽酯衍生物的制备方法
公开(公告)号：US06822111B2
公开(公告)日：2004-11-23
申请号：US10286840
申请日：2002-11-04
申请人： Shigeru Kawahara , Kazutaka Nagashima , Tadashi Takemoto
发明人： Shigeru Kawahara , Kazutaka Nagashima , Tadashi Takemoto
IPC分类号： C07C22900
CPC分类号： C07K5/06113 , A23L27/32
摘要： N-[N-[3-(phenyl having various substituent group(s) on the benzene ring)propyl]-L-&agr;-aspartyl]-L-phenylalanine 1-methyl ester derivatives, which are useful as sweeteners, may be conveniently produced on an industrial scale at a high yield by reductively alkylating aspartame with a 3-(phenyl having specified substituent group(s) on the benzene ring)-2-propenyl aldehyde and hydrogen in the presence of a catalyst and a base.
摘要翻译：丙基] -L-α-天冬氨酰基] -L-苯丙氨酸1-甲酯衍生物，它们可用于甜味剂，可以方便地使用，N- [N- [3-（苯环上具有各种取代基的苯基）通过在催化剂和碱的存在下用3-（苯环上具有特定的取代基的苯基）-2-丙烯基醛和氢还原性地烷基化阿斯巴甜来以高产率工业生产。

4. 发明申请

US20050107473A1 Process for producing tert-leucine 审中-公开
标题翻译：制备叔亮氨酸的方法
公开(公告)号：US20050107473A1
公开(公告)日：2005-05-19
申请号：US10934547
申请日：2004-09-07
申请人： Kazutaka Nagashima , Tadashi Takemoto
发明人： Kazutaka Nagashima , Tadashi Takemoto
IPC分类号： C07C227/42 , C07C229/08 , A61K31/198 , C07C227/34
CPC分类号： C07C227/42 , C07C229/08
摘要： The present invention provides a method of producing tert-leucine, which includes reacting tert-leucine with substituted benzenesulfonic acid represented by the following formula (1) wherein R1 and R2 are each independently a hydrogen atom, an alkyl group or a halogen atom, except a compound wherein R1 and R2 are both hydrogen atoms, in a solvent, to give tert-leucine.substituted benzenesulfonate represented by the following formula (2) wherein R1 and R2 are the same substituents as above, separating the salt by crystallization and then dissociating the salt. According to the present invention, a production method of tert-leucine is provided, which includes forming a tert-leucine salt hardly soluble in a solvent and crystallization thereof to efficiently recover tert-leucine from the solvent.
摘要翻译：本发明提供了一种生产叔亮氨酸的方法，其包括使叔 - 亮氨酸与下式（1）表示的取代苯磺酸反应，其中R 1和R 2各自独立地为氢原子，烷基或卤素原子，除化合物，其中R1和R2都是氢原子，在溶剂中，得到由下式（2）表示的叔 - 亮氨酸取代的苯磺酸盐，其中R 1和R 2是与上述相同的取代基，通过结晶分离盐，然后解离盐。根据本发明，提供了一种叔 - 亮氨酸的制备方法，其包括形成难溶于溶剂的叔 - 亮氨酸盐和结晶，以有效地从溶剂中回收叔 - 亮氨酸。

5. 发明授权

US06933408B2 Intermediate for sweetener with high sweetness and process for producing the same 有权
公开(公告)号：US06933408B2
公开(公告)日：2005-08-23
申请号：US10706083
申请日：2003-11-13
申请人： Shigeru Kawahara , Kenichi Mori , Kazutaka Nagashima , Tadashi Takemoto
发明人： Shigeru Kawahara , Kenichi Mori , Kazutaka Nagashima , Tadashi Takemoto
摘要： The present invention relates to a 3-substituted-phenyl-3-merthylbutyric acid and 3-substituted-phenyl-3-merthylaldehyde derivatives, which are useful in the production of N-[N-[3-(3-hydroxy-4-methoxyphenyl)-3-methylbutyl]-L-α-aspartyl]-L-phenylalanine 1-methyl ester, which is a sweetener with high sweetening potency.

6. 发明申请

US20050175755A1 Process for production of aspartyl dipeptide ester derivative, novel production intermediate therefor, and process for production thereof 审中-公开
标题翻译：天冬氨酰二肽酯衍生物的生产方法，其生产中间体及其生产方法
公开(公告)号：US20050175755A1
公开(公告)日：2005-08-11
申请号：US11105428
申请日：2005-04-14
申请人： Kazutaka Nagashima , Yuuichi Aoki , Tadashi Takemoto , Nao Funakoshi , Eriko Ono
发明人： Kazutaka Nagashima , Yuuichi Aoki , Tadashi Takemoto , Nao Funakoshi , Eriko Ono
IPC分类号： A23L27/30 , C07K5/072 , C07K5/075 , A23L1/236
CPC分类号： C07K5/06113 , A23L27/32
摘要： The present invention relates to a method of manufacturing aspartyl dipeptide ester compounds, which can be used as sweeteners, and aldehydes that can be used in the manufacturing processes.
摘要翻译：本发明涉及可用作甜味剂的天冬氨酰二肽酯化合物的制造方法和可用于制造过程中的醛。

7. 发明授权

US06914151B1 Crystallization processes for the formation of stable crystals of aspartame derivative 失效
标题翻译：用于形成稳定的阿斯巴甜衍生物晶体的结晶过程
公开(公告)号：US06914151B1
公开(公告)日：2005-07-05
申请号：US09830159
申请日：1999-11-01
申请人： Shigeru Kawahara , Akihiro Kishishita , Kazutaka Nagashima , Tadashi Takemoto
发明人： Shigeru Kawahara , Akihiro Kishishita , Kazutaka Nagashima , Tadashi Takemoto
IPC分类号： C07K5/072 , C07K5/075 , C07C229/00
CPC分类号： C07K5/0613
摘要： A crystallization process for forming a stable crystal of N-(3,3-dimethylbutyl)-APM, which comprises using either water or a mixture of water with a lower alcohol as the crystallizing solvent and controlling the crystallization point to 30° C. or above; and another crystallization process therefor, which comprises using either water or a mixture of water with a lower alcohol as the crystallizing solvent and using as the seed crystal a crystal of N-(3,3-dimethylbutyl)-APM exhibiting peculiar peaks of diffracted X-ray at least at diffraction angles (2θ, CuKα ray) of 6.0°, 24.8°, 8.2° and 16.5° to thereby crystallize the above objective crystal preferentially. These crystallization processes enable the constant formation of stable crystals of N-(3,3-dimethylbutyl)-APM at a low cost.
摘要翻译：用于形成N-（3,3-二甲基丁基）-APM的稳定结晶的结晶方法，其包括使用水或水与低级醇的混合物作为结晶溶剂并将结晶点控制在30℃，或以上; 和另一种结晶方法，其包括使用水或水与低级醇的混合物作为结晶溶剂，并且使用表现出衍射X的独特峰的N-（3,3-二甲基丁基）-APM晶种作为晶种至少在6.0°，24.8°，8.2°和16.5°的衍射角（2θ，CuKalpha射线）处，以便优先结晶上述目标晶体。这些结晶过程使得能够以低成本恒定地形成N-（3,3-二甲基丁基）-APM的稳定晶体。

8. 发明授权

US06844465B2 Method for preparing highly stable crystals of aspartame derivative 失效
标题翻译：制备高稳定性阿斯巴甜衍生物晶体的方法
公开(公告)号：US06844465B2
公开(公告)日：2005-01-18
申请号：US10160000
申请日：2002-06-04
申请人： Shigeru Kawahara , Akihiro Kishishita , Kazutaka Nagashima , Tadashi Takemoto
发明人： Shigeru Kawahara , Akihiro Kishishita , Kazutaka Nagashima , Tadashi Takemoto
IPC分类号： C07K5/075 , C07C229/00
CPC分类号： C07K5/0613
摘要： Disclosed in the present application are a method for preparing highly-stable A-type crystals by controlling and maintaining the product temperature of B-type N-(3,3-dimethylbutyl)-APM crystals at 25 to 80° C. under an absolute humidity of 0.203 kg/kg or less environment, thereby effecting crystal transition; and a method for preparing A-type crystals by controlling and maintaining the product temperature of D-type crystals of N-(3,3-dimethylbutyl)-APM at 25 to 80° C. under an absolute humidity of 0.0550 kg/kg or less environment, thereby effecting crystal transition. According to these crystal transition methods, highly stable crystals can be prepared stably and at a low cost.
摘要翻译：本申请中公开了一种通过控制并保持B型N-（3,3-二甲基丁基）-APM晶体在25至80℃下的产物温度在绝对值下制备高度稳定的A型晶体的方法湿度为0.203kg / kg以下的环境，从而进行晶体转变; 以及通过在0.05〜50kg / kg的绝对湿度下在25〜80℃下控制并维持N-（3,3-二甲基丁基）-APM的D-型晶体的产物温度来制备A型晶体的方法或较少的环境，从而进行晶体转变。根据这些晶体转变方法，可以稳定且低成本地制备高度稳定的晶体。

9. 发明授权

US06841183B2 Process for producing aspartame derivatives, process for purifying aspartame derivatives, production intermediates, and process for producing production intermediates 失效
标题翻译：制备阿斯巴甜衍生物的方法，天冬酰苯丙氨酸甲酯衍生物的纯化方法，生产中间体以及生产中间体的生产方法
公开(公告)号：US06841183B2
公开(公告)日：2005-01-11
申请号：US10108426
申请日：2002-03-29
申请人： Kazutaka Nagashima , Shinji Fujita , Yuuichi Aoki , Shigeru Kawahara , Tadashi Takemoto , Eriko Ono
发明人： Kazutaka Nagashima , Shinji Fujita , Yuuichi Aoki , Shigeru Kawahara , Tadashi Takemoto , Eriko Ono
IPC分类号： A23L27/30 , C07D311/20 , C07K5/072 , C07K5/075 , A23L1/236
CPC分类号： C07K5/06113 , A23L27/32 , C07D311/20 , C07K5/0613 , Y02P20/582
摘要： N-[N-[3-(2-hydroxy-substituted phenyl)propyl]-L-α-aspartyl]-L-phenylalanine 1-methyl ester derivatives, which are useful as sweeteners, may be conveniently produced by subjecting a 2-hydroxychroman derivative having various substituents on the benzene ring and aspartame to a reductive alkylation reaction. These compounds may be purified by subjecting such a derivative containing one or more impurities to a crystallization step to crystallize the same. Further, there are provided a process for producing dialkoxychroman derivatives useful as intermediates for the production of such aspartame derivatives in the above process, and novel dialkoxychroman derivatives thus produced, which are excellent as the production intermediate.
摘要翻译：可用作甜味剂的N- [N- [3-（2-羟基取代的苯基）丙基] -L-α-天冬氨酰基] -L-苯丙氨酸1-甲酯衍生物可以方便地通过使2- 在苯环上具有各种取代基的羟基苯并二氢吡喃衍生物和阿斯巴甜进行还原烷基化反应。这些化合物可以通过将含有一种或多种杂质的衍生物进行结晶步骤进行结晶来纯化。此外，提供了用作上述方法中用于生产这种阿斯巴甜衍生物的中间体的二烷氧基苯并二氢吡喃衍生物的方法，以及如此生产的新型二烷氧基苯并二氢吡喃衍生物，其作为制备中间体是优异的。

10. 发明授权

US06818243B2 Crystals of aspartame derivative 失效
标题翻译：阿斯巴甜衍生物晶体
公开(公告)号：US06818243B2
公开(公告)日：2004-11-16
申请号：US10183652
申请日：2002-06-28
申请人： Kazutaka Nagashima , Yuuichi Aoki , Eriko Ono , Tadashi Takemoto
发明人： Kazutaka Nagashima , Yuuichi Aoki , Eriko Ono , Tadashi Takemoto
IPC分类号： A23L1236
CPC分类号： C07K5/06113 , A23L27/32
摘要： N-[N-[3-(3-hydroxy-4-methoxyphenyl)propyl]-L-&agr;-aspartyl]-L-phenylalanine 1-methyl ester useful as a sweetener with a high potency of sweetness, is provided in the crystalline form having a high stability and a good purity which is favorable as a commercial product.
摘要翻译：在结晶中提供了可用作甜度高的甜味剂的N- [N- [3-（3-羟基-4-甲氧基苯基）丙基] -L-α-天冬氨酰基] -L-苯丙氨酸1-甲基酯形式具有高稳定性和良好的纯度，作为商业产品是有利的。

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