KR101088020B1 - 아데포비어 디피복실의 dh형 결정, 이의 제조방법, 및 이를 포함하는 항바이러스제 조성물 - Google Patents
아데포비어 디피복실의 dh형 결정, 이의 제조방법, 및 이를 포함하는 항바이러스제 조성물 Download PDFInfo
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- KR101088020B1 KR101088020B1 KR1020090026612A KR20090026612A KR101088020B1 KR 101088020 B1 KR101088020 B1 KR 101088020B1 KR 1020090026612 A KR1020090026612 A KR 1020090026612A KR 20090026612 A KR20090026612 A KR 20090026612A KR 101088020 B1 KR101088020 B1 KR 101088020B1
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- South Korea
- Prior art keywords
- adefovir difficile
- adefovir
- crystals
- difficile
- solvent
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- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic Table
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Abstract
Description
결정구조 | X-선 회절(2θ) | 시차주사열량 |
DH 결정형 | 7.84, 8.49, 9.65, 12.43, 14.08, 14.31, 14.69, 15.5, 16.06, 17.14, 17.66, 18.35, 19.10, 19.45, 19.70, 20.34, 20.82, 21.82, 22.11, 22.86, 23.55, 24.46, 25.06. 26.45, 27.03, 27.66, 28.37, 29.09, 29.77 | 71.6 ℃ |
무수결정형 (결정형 1) |
6.9, 11.8, 12.7, 15.7, 17.2, 20.7, 21.5, 22.5, 23.3 | 102 ℃ |
수화물결정형 (결정형 2) |
9.6, 16.3, 18.3, 18.9, 19.7, 21.0-21.3, 21.4, 22.0, 24.3, 27.9, 30.8, 32.8 | 73 ℃ |
용매화물결정형 (결정형 3) |
8.1, 8.7, 14.1, 16.5, 17.0, 19.4, 21.1, 22.6, 23.4, 24.2, 25.4, 30.9 | 85 ℃ |
Claims (12)
- 삭제
- 삭제
- 삭제
- 삭제
- 아데포비어 디피복실을 n-부틸알콜의 결정용매에 용해시킨 후, -10℃ 내지 30℃ 온도에서 방치하여 석출된 고체를 수득하는,X-선 회절분석도에서 피크 강도가 200 이상을 갖는 회절각(2θ)의 값이 7.84, 8.49, 9.65, 12.43, 14.08, 14.31, 14.69, 15.5, 16.06, 17.14, 17.66, 18.35, 19.10, 19.45, 19.70, 20.34, 20.82, 21.82, 22.11, 22.86, 23.55, 24.46, 25.06. 26.45, 27.03, 27.66, 28.37, 29.09, 29.77인 하기 화학식 1로 표시되는 아데포비어 디피복실의 DH형 결정의 제조방법.[화학식 1]
- 청구항 5에 있어서,상기 결정용매는 n-부틸알콜의 단독 용매로 사용하거나, 또는 n-부틸알콜에 C3-C7 케톤, C2-C7 포화 알코올, C2-C7 에테르, N,N-디메틸포름아미드(DMF), N,N-디메틸아세트아미드(DMAC), N,N'-디메틸프로필렌우레아(DMPU), C3-C7 알킬 아세테이트, C5-C10 탄화수소, C1-C4 클로로탄화수소 및 C3-C7 니트릴 중에서 선택된 조용매가 10 내지 50 부피% 포함된 혼합용매를 사용하는 것을 특징으로 하는 아데포비어 디피복실의 DH형 결정의 제조방법.
- 청구항 5에 있어서,상기 n-부틸알콜에 용해되는 아데포비어 디피복실은 무정형, 결정형, 무수형, 또는 용매화물 형태의 아데포비어 디피복실인 것을 특징으로 하는 아데포비어 디피복실의 DH형 결정의 제조방법.
- 청구항 5에 있어서,상기 방치는 탄소수 3 내지 7의 케톤, 탄소수 2 내지 7의 알콜, 탄소수 2 내지 7의 에테르, 탄소수 3 내지 7의 에스테르, 및 탄소수 3 내지 7의 아미드류 중에서 선택된 단독 용매 또는 혼합용매가 추가로 포함되는 조건에서 수행하는 것을 특징으로 하는 아데포비어 디피복실의 DH형 결정의 제조방법.
- 청구항 5에 있어서,상기 용해는 20℃ 내지 150℃ 온도 범위에서 수행하는 것을 특징으로 하는 아데포비어 디피복실 결정의 제조방법.
- 상기 청구항 5 내지 9항 중에서 선택된 어느 한 항의 방법으로 얻어진 아데포비어 디피복실의 DH형 결정이 함유된 것을 특징으로 하는 항바이러스제용 약제조성물.
- 청구항 5 또는 6항에 있어서,결정격자 구조내에 함유된 결정용매의 함량이 0.5 당량 범위인 아데포비어 디피복실 결정의 제조방법.
- 청구항 5에 있어서,시차주사 열량 기록도 (Differential Scanning Calorimeter Thermogram)에서 최대 흡열피크가 71.6℃에 존재하는 아데포비어 디피복실의 DH형 결정의 제조방법.
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KR1020090026612A KR101088020B1 (ko) | 2009-03-27 | 2009-03-27 | 아데포비어 디피복실의 dh형 결정, 이의 제조방법, 및 이를 포함하는 항바이러스제 조성물 |
PCT/KR2009/002685 WO2010110506A1 (en) | 2009-03-27 | 2009-05-21 | Dh-type crystalline form of adefovir dipivoxil, preparing method thereof, and pharmaceutical composition for antiviral agent comprising the same |
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