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    Crystallization processes for the formation of stable crystals of aspartame derivative
    82.
    发明授权
    Crystallization processes for the formation of stable crystals of aspartame derivative 失效
    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。

    Method for preparing highly stable crystals of aspartame derivative
    83.
    发明授权
    Method for preparing highly stable crystals of aspartame derivative 失效
    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。

    Crystals of aspartame derivative
    85.
    发明授权
    Crystals of aspartame derivative 失效
    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。

    Arylpropyl aldehyde derivatives, processes for producing the same, and methods of using the same
    89.
    发明授权
    Arylpropyl aldehyde derivatives, processes for producing the same, and methods of using the same 失效
    芳基丙醛衍生物，其制备方法及其使用方法

    公开(公告)号：US06689902B2

    公开(公告)日：2004-02-10

    申请号：US10197808

    申请日：2002-07-19

    申请人： Kenichi Mori ,  Shigeru Kawahara ,  Tadashi Takemoto

    发明人： Kenichi Mori ,  Shigeru Kawahara ,  Tadashi Takemoto

    IPC分类号： C07C5900

    CPC分类号： C07C69/734 ,  C07C45/41 ,  C07C47/27 ,  C07C47/277 ,  C07C51/367 ,  C07C59/64 ,  C07C59/52

    摘要： 3-(3-Methyl-4-hydroxyphenyl)-3-methylbutyl aldehyde may be produced from 3-(3-methyl-4-hydroxyphenyl)-3-methylbutyric acid by converting the carboxyl group into a formyl group. N-[N-[3-(3-methyl-4-hydroxyphenyl)-3-methylbutyl]-L-&agr;-aspartyl]-L-phenylalanine 1-methyl ester, which is useful as a sweetener having a high potency of sweetness, can be easily and efficiently prepared on an industrial production from such an aldehyde derivative, via a reductive alkylation reaction with aspartame. Therefore, 3-(3-Methyl-4-hydroxyphenyl)-3-methylbutyl aldehyde is extremely excellent as an intermediate for the production of N-[N-[3-(3-methyl-4-hydroxyphenyl)-3-methylbutyl]-L-&agr;-aspartyl]-L-phenylalanine 1-methyl ester. The above butyric acid derivative is a novel compound, which can be easily produced by subjecting 3-(3-methyl-4-methoxyphenyl)-3-methylbutyric acid obtained by the reaction of 2-methoxytoluene with 3-methylcrotonic acid, to a reaction for converting a methoxy group into a hydroxyl group. The present invention further provides several novel compounds useful as a production intermediate, such as the above aldehyde derivative and the like.

    摘要翻译： 3-（3-甲基-4-羟基苯基）-3-甲基丁醛可以通过将羧基转变为甲酰基而由3-（3-甲基-4-羟基苯基）-3-甲基丁酸制备。 N- [N- [3-（3-甲基-4-羟基苯基）-3-甲基丁基] -L-α-天冬氨酰基] -L-苯丙氨酸1-甲基酯，其可用作具有高效能甜度的甜味剂 可以通过这种醛衍生物通过与阿斯巴甜的还原烷基化反应在工业生产上容易且有效地制备。 因此，3-（3-甲基-4-羟基苯基）-3-甲基丁基醛作为制备N- [N- [3-（3-甲基-4-羟基苯基）-3-甲基丁基] -L-α-天冬氨酰基] -L-苯丙氨酸1-甲酯。上述丁酸衍生物是一种新型化合物，其可以通过使3-（3-甲基-4-甲氧基苯基）-3-甲基丁酸得到 通过2-甲氧基甲苯与3-甲基巴豆酸的反应，将甲氧基转化成羟基的反应。本发明还提供了几种可用作生产中间体的新型化合物，例如上述醛衍生物等。