IPC분류정보
국가/구분 |
United States(US) Patent
등록
|
국제특허분류(IPC7판) |
|
출원번호 |
US-0830159
(1999-11-01)
|
우선권정보 |
JP-10/310225 (1998-10-30); JP-10/310226 (1998-10-30) |
국제출원번호 |
PCT//JP99/06082
(2001-06-27)
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§371/§102 date |
20010627
(20010627)
|
국제공개번호 |
WO00//26234
(2000-05-11)
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발명자
/ 주소 |
- Kawahara, Shigeru
- Kishishita, Akihiro
- Nagashima, Kazutaka
- Takemoto, Tadashi
|
출원인 / 주소 |
|
대리인 / 주소 |
Oblon, Spivak, McClelland, Maier &
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인용정보 |
피인용 횟수 :
2 인용 특허 :
14 |
초록
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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,
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.
대표청구항
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1. A method for preparing A-type crystals of N-[N-(3,3-dimethylbutyl)-L-α-aspartyl]-L-phenylalanine methyl ester, comprising:crystallizing N-[N-(3,3-dimethylbutyl)-L-α-aspartyl]-L-phenylalanine methyl ester from a solution comprising N-[N-(3,3-dimethylbutyl)-L-α-aspartyl]-L-phenylalanine methyl este
1. A method for preparing A-type crystals of N-[N-(3,3-dimethylbutyl)-L-α-aspartyl]-L-phenylalanine methyl ester, comprising:crystallizing N-[N-(3,3-dimethylbutyl)-L-α-aspartyl]-L-phenylalanine methyl ester from a solution comprising N-[N-(3,3-dimethylbutyl)-L-α-aspartyl]-L-phenylalanine methyl ester and a solvent, to obtain A-type crystals of N-[N-(3,3-dimethylbutyl)-L-α-aspartyl]-L-phenylalanine methyl ester, wherein said solvent is selected from the group consisting of water and mixtures of water and a lower alcohol, wherein said crystallizing is carried out such that the temperature of said solution is maintained above 47° C. until onset of nucleation of said A-type N-[N-(3,3-dimethylbutyl)-L-α-aspartyl]-L-phenylalanine methyl ester. 2. The method of claim 1, wherein said solvent is a mixture of water and methanol.3. The method of claim 1, wherein said methanol is present in said solvent in an amount of 15 wt. % or less, based on the total weight of said solvent.4. The method of claim 1, wherein said solvent is water.5. A method for preparing A-type crystals of N-[N-(3,3-dimethylbutyl)-L-α-aspartyl]-L-phenylalanine methyl ester, comprising:crystallizing N-[N-3,3-dimethylbutyl)-L-α-aspartyl]-L-phenylalanine methyl ester from a solution comprising N-[N-(3,3-dimethylbutyl)-L-α-aspartyl]-L-phenylalanine methyl ester and a solvent, to obtain A-type crystals of N-[N-(3,3-dimethylbutyl)-L-α-aspartyl]-L-phenylalanine methyl ester, wherein said solvent is selected from the group consisting of water and mixtures of water and a lower alcohol, wherein said crystallizing is carried out in the presence of seed crystals of A-type N-[N-(3,3-dimethylbutyl)-L-α-aspartyl]-L-phenylalanine methyl ester. 6. The method of claim 5, wherein said solvent is a mixture of water and methanol.7. The method of claim 6, wherein said methanol is present in said solvent in an amount of 15 wt. % or less, based on the total weight of said solvent.8. The method of claim 5, wherein said solvent is water.9. The method of claim 1, wherein said A-type crystals of N-[N-(3,3-dimethylbutyl)-L-α-aspartyl]-L-phenylalanine methyl ester exhibit a CuKα x-ray diffraction pattern having characteristic peaks expressed in degrees 2θ at 6.0°, 8.2°, 16.5°, and 24.8°.10. The method of claim 1, wherein said A-type crystals of N-[N-(3,3-dimethylbutyl)-L-α-aspartyl]-L-phenylalanine methyl ester exhibit a CuKα x-ray diffraction pattern having characteristic peaks expressed in degrees 2θ at 6.0°, 8.2°, 16.5°, and 24.8°.11. The method of claim 5, wherein said seed crystals of A-type crystals of N-[N-(3,3-dimethylbutyl)-L-α-aspartyl]-L-phenylalanine methyl ester exhibit a CuKα x-ray diffraction pattern having characteristic peaks expressed in degrees 20 at 6.0°, 8.2°, 16.5°, and 24.8°.12. A method for preparing A-type crystals of N-[N-(3,3-dimethylbutyl)-L-α-aspartyl]-L-phenylalanine methyl ester, comprising:crystallizing N? (N-(3,3-dimethylbutyl)-L-α-aspartyl]-L-phenylalanine methyl ester from a solution comprising N-[N-(3,3-dimethylbutyl)-L-α-aspartyl]-L-phenylalanine methyl ester and a solvent, to obtain A-type crystals of N-[N-(3,3-dimethylbutyl)-L-α-aspartyl]-L-phenylalanine methyl ester, wherein said solvent is selected from the group consisting of water and mixtures of water and a lower alcohol, wherein said crystallizing is carried out such that the temperature of said solution is maintained at 40° C. to 50° C. until onset of nucleation of said A-type N-[N-(3,3-dimethylbutyl)-L-α-aspartyl]-L-phenylalanine methyl ester. 13. The method of claim 12, wherein said solvent is a mixture of water and methanol.14. The method of claim 13, wherein said methanol is present in said solvent in an amount of 15 wt. % or less, based on the total weight of said solvent.15. The method of claim 12, wherein said solvent is water.16. The method of claim 12, wherein said A-type crystals of N-[N-(3,3-dimethylbutyl)-L-α-aspartyl]-L-phenylalanine methyl ester exhibit a CuKα x-ray diffraction pattern having characteristic peaks expressed in degrees 2θ at 6.0°, 8.2°, 16.5°, and 24.8°.
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