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1. 发明授权

US5304671A Method for recovery of .alpha.-L-aspartyl-L-phenylalanine methyl ester, L-phenylalanine and L-aspartic acid 失效
标题翻译： α-天冬氨酰-L-苯丙氨酸甲酯，L-苯丙氨酸和L-天冬氨酸的回收方法
公开(公告)号：US5304671A
公开(公告)日：1994-04-19
申请号：US925039
申请日：1992-08-05
申请人： Sou Abe , Shinichi Kishimoto , Tadashi Takemoto , Toshihisa Kato , Satoshi Kumon
发明人： Sou Abe , Shinichi Kishimoto , Tadashi Takemoto , Toshihisa Kato , Satoshi Kumon
IPC分类号： C07K1/14 , C07C227/40 , C07C229/24 , C07C229/36 , C07K5/072 , C07K5/075 , C07C229/34
CPC分类号： C07K5/0613 , C07C227/40
摘要： A method for the recovery of .alpha.-L-aspartyl-L-phenylalanine methyl ester, L-phenylalanine and L-aspartic acid from the mother liquor obtained by the solid-liquid separation of a suspension of .alpha.-L-aspartyl-L-phenylalanine methyl ester crystals is disclosed.
摘要翻译：一种从母液中回收（α）-L-天冬氨酰基-L-苯丙氨酸甲酯，L-苯丙氨酸和L-天冬氨酸的方法，该方法是通过固液分离（α）-L-天冬氨酰基公开了L-苯丙氨酸甲酯晶体。

2. 发明授权

US5292923A Method of preparing .alpha.-l-aspartyl-l-phenylalanine methyl ester hydrochloride 失效
标题翻译：制备α1-天冬氨酰-1-苯丙氨酸甲酯盐酸盐的方法
公开(公告)号：US5292923A
公开(公告)日：1994-03-08
申请号：US886101
申请日：1992-05-21
申请人： Toshihisa Kato , Shinichi Kishimoto , Hideo Takeda , Mikiya Kano , Tadashi Takemoto
发明人： Toshihisa Kato , Shinichi Kishimoto , Hideo Takeda , Mikiya Kano , Tadashi Takemoto
IPC分类号： C07K1/02 , C07K1/14 , C07K5/075 , C07C229/00
CPC分类号： C07K5/0613
摘要： A method of preparing .varies.-L-aspartyl-L-phenylalanine methyl ester hydrochloride (.varies.-APM.HCL) from a reaction mixture of N-formyl-L-aspartic acid anhydride and L-phenylalanine methyl ester (PM), wherein .alpha.-APM.HCl is produced without isolating an intermediate by solid-liquid separation during the course of the reaction process.
摘要翻译：从N-甲酰基-L-天冬氨酸酐和L-苯丙氨酸甲酯（的反应混合物）中制备（变化为）-L-天冬氨酰基-L-苯丙氨酸甲酯盐酸盐（（根据-APM.HCL变化））的方法 PM），其中（α）-APM.HCl是在反应过程中通过固液分离而不分离中间体的。

3. 发明授权

US5501712A Method for crystallization of .alpha.-L-aspartyl-L-phenylalanine methyl ester 失效
公开(公告)号：US5501712A
公开(公告)日：1996-03-26
申请号：US326953
申请日：1994-10-21
申请人： Sou Abe , Shinichi Kishimoto
发明人： Sou Abe , Shinichi Kishimoto
IPC分类号： A23L27/30 , C07K1/14 , C07K5/072 , C07K5/075 , C07C229/00 , B01D9/02
CPC分类号： C07K5/0613 , Y10S530/801
摘要： The problems in crystallization of .alpha.-L-aspartyl-L-phenylalanine methyl ester, namely, problems in crystal slurry properties in solid-liquid separation, scaling at heat transfer surfaces, and the like, are solved by a method for crystallization of .alpha.-L-aspartyl-L-phenylalanine methyl ester which comprises cooling a solution of .alpha.-L-aspartyl-L-phenylalanine methyl ester by indirect heat exchange with a coolant while stirring, wherein the solution is cooled by circulating a coolant while continuously adding an aqueous solution of .alpha.-L-aspartyl-L-phenylalanine methyl ester dropwise to a crystallizing solution of .alpha.-L-aspartyl-L-phenylalanine methyl ester having a temperature difference of not greater than 20.degree. C. from the coolant, thereby to keep a temperature difference of not greater than 20.degree. C. between the coolant and the crystallizing solution.

4. 发明授权

US5425787A Method for crystallization of .alpha.-L-aspartyl-L-phenylalanine methyl ester 失效
标题翻译： α-L-天冬氨酰-L-苯丙氨酸甲酯的结晶方法
公开(公告)号：US5425787A
公开(公告)日：1995-06-20
申请号：US203472
申请日：1994-02-28
申请人： Sou Abe , Shinichi Kishimoto
发明人： Sou Abe , Shinichi Kishimoto
IPC分类号： A23L27/30 , C07K1/14 , C07K5/072 , C07K5/075 , C07C229/00
CPC分类号： C07K5/0613 , Y10S530/801
摘要： The problems in crystallization of .alpha.-L-aspartyl-L-phenylalanine methyl ester, namely, problems in crystal slurry properties in solid-liquid separation, scaling at heat transfer surfaces, and the like, are solved by a method for crystallization of .alpha.-L-aspartyl-L-phenylalanine methyl ester which comprises cooling a solution of .alpha.-L-aspartyl-L-phenylalanine methyl ester by indirect heat exchange with a coolant while stirring, wherein the solution is cooled by circulating a coolant while continuously adding an aqueous solution of .alpha.-L-aspartyl-L-phenylalanine methyl ester dropwise to a crystallizing solution of .alpha.-L-aspartyl-L-phenylalanine methyl ester having a temperature difference of not greater than 20.degree. C. from the coolant, thereby to keep a temperature difference of not greater than 20.degree. C. between the coolant and the crystallizing solution.
摘要翻译： α-L-天冬氨酰-L-苯丙氨酸甲酯的结晶问题，即固液分离中的结晶浆料性质，传热表面的结垢等问题，通过α - L-天冬氨酰基-L-苯丙氨酸甲酯，其包括通过在搅拌下与冷却剂间接热交换来冷却α-L-天冬氨酰基-L-苯丙氨酸甲酯的溶液，其中通过循环冷却剂冷却溶液，同时连续加入水将α-L-天冬氨酰基-L-苯丙氨酸甲酯的溶液滴加到冷冻剂的温度差不大于20℃的α-L-天冬氨酰基-L-苯丙氨酸甲酯的结晶溶液中，从而保持冷却液和结晶溶液之间的温差不超过20℃。

5. 发明授权

US4606854A Method of preparing .alpha.-L-aspartyl-L-phenylalanine methyl ester and its hydrochloride 失效
标题翻译：制备α-L-天冬氨酰-L-苯丙氨酸甲酯及其盐酸盐的方法
公开(公告)号：US4606854A
公开(公告)日：1986-08-19
申请号：US611531
申请日：1984-05-17
申请人： Yoichi Ozawa , Shinichi Kishimoto , Emiko Shinohara , Tadashi Takemoto , Chikahiko Eguchi
发明人： Yoichi Ozawa , Shinichi Kishimoto , Emiko Shinohara , Tadashi Takemoto , Chikahiko Eguchi
IPC分类号： C07K1/113 , C07K1/02 , C07K5/06 , C07K5/075
CPC分类号： C07K5/0613
摘要： A method for preparing .alpha.-L-aspartyl-L-phenylalanine methyl ester and its hydrochloride which comprises dissolving .alpha.-L-aspartyl-L-phenylalanine dimethyl ester in a mixture of 0-10% (v/v) methanol, 8-55% (v/v) of concentrated hydrochloric acid, and water (remainder) to a concentration of 0.01 mol/dl to 0.30 mol/dl; holding the resulting solution at one or more temperatures between 0.degree. and 60.degree. C. for a time sufficient for crystals of .alpha.-L-aspartyl-L-phenylalanine methyl ester hydrochloride to precipitate out, and isolating the crystals. The hydrochloride may then be treated with alkali to yield .alpha.-L-aspartyl-L-phenylalanine methyl ester.
摘要翻译：制备α-L-天冬氨酰-L-苯丙氨酸甲酯及其盐酸盐的方法，其包括将α-L-天冬氨酰基-L-苯丙氨酸二甲酯溶解在0-10％（v / v）甲醇，8-55 ％（v / v）浓盐酸和水（剩余物）至0.01mol / dl至0.30mol / dl的浓度; 将所得溶液保持在0℃至60℃之间的一个或多个温度下，足以使α-L-天冬氨酰基-L-苯丙氨酸甲酯盐酸盐的晶体沉淀出来，并分离晶体。然后用碱处理盐酸盐，得到α-L-天冬氨酰基-L-苯丙氨酸甲酯。

6. 发明授权

US4618695A Method of preparing methyl ester and its hydrochloride 失效
标题翻译：制备甲酯及其盐酸盐的方法
公开(公告)号：US4618695A
公开(公告)日：1986-10-21
申请号：US611548
申请日：1984-05-17
申请人： Yoichi Ozawa , Shinichi Kishimoto , Emiko Shinohara , Tadashi Takemoto , Chikahiko Eguchi
发明人： Yoichi Ozawa , Shinichi Kishimoto , Emiko Shinohara , Tadashi Takemoto , Chikahiko Eguchi
IPC分类号： C07K5/075 , C07C101/02
CPC分类号： C07K5/0613
摘要： A method of preparing .alpha.-L-phenylalanine methyl ester and its hydrochloride, which comprises dissolving .alpha.-L-aspartyl-L-phenylalanine .beta.-methyl ester in a methanol/hydrochloric acid mixture solvent which contains, when hydrochloric acid is expressed in terms of concentrated hydrochloric acid and water, 0 to 20% by volume of methanol, 8 to 55% by volume of concentrated hydrochloric acid and water (balance) in a concentration from 0.01 mol/dl to 0.3 mol/dl; holding the solution at 0.degree. to 60.degree. C. to effect intramolecular ester exchange reaction and crystallize out the formed .alpha.-L-aspartyl-L-phenylalanine methyl ester as its hydrochloride; isolating the hydrochloride; and obtaining, when required, the free ester by neutralization with an alkali, is disclosed.
摘要翻译：一种制备α-L-苯丙氨酸甲酯及其盐酸盐的方法，其包括将α--L-天冬氨酰基-L-苯丙氨酸β-甲酯溶于甲醇/盐酸混合物溶剂中，所述溶剂含有当盐酸以浓盐酸和水，0至20体积％甲醇，8至55体积％浓盐酸和水（余量），浓度为0.01mol / dl至0.3mol / dl; 将溶液保持在0〜60℃，进行分子内酯交换反应，结晶形成的α-L-天冬氨酰-L-苯丙氨酸甲酯为盐酸盐; 分离盐酸盐; 并且当需要时通过用碱中和获得游离酯。

7. 发明授权

US5393915A Method of preparing .alpha.-L-aspartyl-L-phenylalanine methyl ester or its hydrochloride salt 失效
标题翻译：制备α-L-天冬氨酰基-L-苯丙氨酸甲酯或其盐酸盐的方法
公开(公告)号：US5393915A
公开(公告)日：1995-02-28
申请号：US153490
申请日：1993-11-17
申请人： Takehiko Kataoka , Akihiko Yasaki , Shinichi Kishimoto , Toshihisa Kato
发明人： Takehiko Kataoka , Akihiko Yasaki , Shinichi Kishimoto , Toshihisa Kato
IPC分类号： C07K1/14 , C07K1/34 , C07K5/072 , C07K5/075 , C07C229/34
CPC分类号： C07K5/0613
摘要： A method for the solid-liquid separation of a suspension of .alpha.-L-aspartyl-L-phenylalanine methyl ester (.alpha.-APM) or its hydrochloride salt (.alpha.-APM.HCl), wherein an aqueous suspension of .alpha.-L-aspartyl-L-phenylalanine methyl ester or its hydrochloride salt is subjected to continuous separation by vacuum filtration.
摘要翻译：一种固定液体分离α-L-天冬氨酰基-L-苯丙氨酸甲酯（α-APM）或其盐酸盐（α-APM.HCl）的悬浮液的方法，其中将α-L-天冬氨酰基 -L-苯丙氨酸甲酯或其盐酸盐通过真空过滤进行连续分离。

8. 发明授权

US5391810A Method of crystallizing .alpha.-L-aspartyl-L-phenylalanine methyl ester 失效
标题翻译： α-L-天冬氨酰-L-苯丙氨酸甲酯的结晶方法
公开(公告)号：US5391810A
公开(公告)日：1995-02-21
申请号：US121569
申请日：1993-09-16
申请人： So Abe , Shinichi Kishimoto , Toshihisa Kato , Hideo Takeda
发明人： So Abe , Shinichi Kishimoto , Toshihisa Kato , Hideo Takeda
IPC分类号： C07K5/072 , C07K5/075 , C07C101/02
CPC分类号： C07K5/0613
摘要： In crystallizing .alpha.-APM from a water solution or a mixed solvent solution of water and a lower alcohol in a crystallizer, the pressure in the crystallizer is held at not higher than atmospheric pressure, a water or water/alcohol mixed solution of .alpha.-APM is fed into the crystallizer with stirring so that the solvent is vaporized, and the crystallization solution is cooled and crystallized by the latent heat of vaporization or is heated so as to prevent supercooling.
摘要翻译：在结晶器中从水溶液或水和低级醇的混合溶剂溶液中结晶α-APM时，将结晶器中的压力保持在不高于大气压的水溶液或水/乙醇混合的α-APM溶液在搅拌下进料到结晶器中，使溶剂蒸发，并将结晶溶液冷却并通过蒸发潜热结晶或加热，以防止过冷。

9. 发明授权

US5248806A Method of 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：US5248806A
公开(公告)日：1993-09-28
申请号：US885977
申请日：1992-05-20
申请人： Shinichi Kishimoto , So Abe , Toshihisa Kato
发明人： Shinichi Kishimoto , So Abe , Toshihisa Kato
IPC分类号： C07K1/02 , C07K1/14 , C07K5/06 , C07K5/072 , C07K5/075
CPC分类号： C07K5/0613
摘要： An acid addition salt of .alpha.-APM is dissolved or suspended in an aqueous medium at 50.degree. C. or lower at a pH of 3 or less and a concentration of the salt of 3 wt.% or more (solution A). A liquid having a pH of 3 or more and containing or not containing .alpha.-APM is prepared (solution B) and gradually mixed with solution A with stirring. The temperature of the liquid mixture is kept to be 40.degree. C. or lower and the pH value of the mixture is kept at 3 or more, optionally adding a base thereto, whereby crystals of .alpha.-APM are precipitated out.

10. 发明授权

US5266719A Method of preparing .alpha.-L-aspartyl-L-phenylalanine methyl ester 失效
标题翻译：制备α-L-天冬氨酰-L-苯丙氨酸甲酯的方法
公开(公告)号：US5266719A
公开(公告)日：1993-11-30
申请号：US885766
申请日：1992-05-20
申请人： Shinichi Kishimoto , Kimiyasu Sakamoto , So Abe , Toshihisa Kato
发明人： Shinichi Kishimoto , Kimiyasu Sakamoto , So Abe , Toshihisa Kato
IPC分类号： C07K1/02 , C07K1/14 , C07K5/072 , C07K5/075 , C07C229/00
CPC分类号： C07K5/0613
摘要： In neutralizing an acid addition salt of .alpha.-APM in an aqueous medium, the .alpha.-APM concentration in the neutralized liquid is controlled to fall within the range of from 3 to 10 wt. % at the finish of neutralization. Then, the liquid is heated to 50.degree. to 80.degree. C. and neutralization is effected with stirring to the isoelectric point of .alpha.-APM; or after the neutralization, the neutralized liquid is heated. The neutralized liquid is thereafter cooled with or without stirring so that crystals of .alpha.-APM are precipitated.

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