CN1871249A - 热稳定的结晶盐酸表柔比星及其制造方法 - Google Patents
热稳定的结晶盐酸表柔比星及其制造方法 Download PDFInfo
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- CN1871249A CN1871249A CNA2004800191272A CN200480019127A CN1871249A CN 1871249 A CN1871249 A CN 1871249A CN A2004800191272 A CNA2004800191272 A CN A2004800191272A CN 200480019127 A CN200480019127 A CN 200480019127A CN 1871249 A CN1871249 A CN 1871249A
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- epirubicin hydrochloride
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H15/00—Compounds containing hydrocarbon or substituted hydrocarbon radicals directly attached to hetero atoms of saccharide radicals
- C07H15/20—Carbocyclic rings
- C07H15/24—Condensed ring systems having three or more rings
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P35/00—Antineoplastic agents
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- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
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- Plural Heterocyclic Compounds (AREA)
Abstract
Description
衍射角 | 相对强度 |
2Θ | P(%) |
5.236 | 9.8 |
9.212 | 12.5 |
13.732 | 15.5 |
16.446 | 4.8 |
18.234 | 5 |
21.114 | 9.7 |
22.529 | 25.5 |
24.071 | 29.9 |
25.879 | 18.4 |
27.762 | 16.5 |
29.757 | 10.1 |
34.392 | 4.4 |
38.157 | 13.1 |
44.293 | 5.9 |
64.699 | 7.7 |
77.815 | 100 |
2Θ | d(A) | BG | 峰 | P(%) | 面积 | FWHM |
5.236 | 16.8641 | 22 | 415 | 9.8 | 122 | 0.234 |
9.212 | 9.5918 | 15 | 531 | 12.5 | 207 | 0.311 |
13.732 | 6.4434 | 40 | 658 | 15.5 | 211 | 0.256 |
16.446 | 5.3855 | 122 | 204 | 4.8 | 115 | 0.449 |
18.234 | 4.8614 | 74 | 214 | 5 | 105 | 0.39 |
21.114 | 4.2042 | 43 | 411 | 9.7 | 233 | 0.453 |
22.529 | 3.9433 | 323 | 1084 | 25.5 | 405 | 0.299 |
24.071 | 3.6941 | 102 | 1272 | 29.9 | 422 | 0.265 |
25.879 | 3.44 | 75 | 780 | 18.4 | 348 | 0.357 |
27.762 | 3.2108 | 71 | 701 | 16.5 | 319 | 0.363 |
29.757 | 2.9999 | 109 | 428 | 10.1 | 150 | 0.279 |
34.392 | 2.6055 | 67 | 186 | 4.4 | 101 | 0.434 |
38.157 | 2.3566 | 114 | 558 | 13.1 | 196 | 0.28 |
44.293 | 2.0433 | 78 | 249 | 5.9 | 91 | 0.292 |
64.699 | 1.4395 | 19 | 328 | 7.7 | 130 | 0.316 |
77.815 | 1.2264 | 41 | 4250 | 100 | 1817 | 0.342 |
2-Θ | d(A) | BG | 峰 | P(%) | 面积 | FWHM |
38.236 | 2.3519 | 8 | 1750 | 47.7 | 585 | 0.267 |
44.453 | 2.0363 | 6 | 802 | 21.9 | 302 | 0.301 |
64.825 | 1.4371 | 7 | 373 | 10.2 | 141 | 0.301 |
77.955 | 1.2246 | 21 | 3667 | 100 | 1520 | 0.331 |
82.139 | 1.1725 | 12 | 277 | 7.6 | 120 | 0.344 |
月数 | 加速储存条件40℃±2℃ | ||||||||
ESP01批 | ESP02批 | ESP03批 | |||||||
测定* | 阿霉素酮 | 总杂质 | 测定* | 阿霉素酮 | 总杂质 | 测定* | 阿霉素酮 | 总杂质 | |
最初 | 99.2 | 0.04 | 0.39 | 99.3 | 未检测 | 0.37 | 99.0 | 0.06 | 0.42 |
3 | 99.1 | 0.07 | 0.44 | 99.0 | 0.06 | 0.44 | 99.1 | 0.12 | 0.48 |
6 | 99.1 | 0.12 | 0.50 | 99.0 | 0.14 | 0.51 | 99.0 | 0.15 | 0.53 |
月数 | 加速储存条件40℃±2℃ | ||||||||
ESP04批 | ESP05批 | ESP063批 | |||||||
测定* | 阿霉素酮 | 总杂质 | 测定* | 阿霉素酮 | 总杂质 | 测定* | 阿霉素酮 | 总杂质 | |
最初 | 98.8 | 0.17 | 0.42 | 99.0 | 0.21 | 0.45 | 99.2 | 0.07 | 0.42 |
3 | 94.3 | 2.1 | 2.7 | 94.0 | 2.4 | 3.0 | 95.1 | 1.8 | 2.4 |
6 | 89.0 | 6.0 | 7.6 | 90.1 | 5.8 | 7.7 | 90.2 | 5.4 | 6.9 |
Claims (14)
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US48413203P | 2003-07-02 | 2003-07-02 | |
US60/484,132 | 2003-07-02 |
Publications (2)
Publication Number | Publication Date |
---|---|
CN1871249A true CN1871249A (zh) | 2006-11-29 |
CN100412084C CN100412084C (zh) | 2008-08-20 |
Family
ID=34062027
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CNB2004800191272A Expired - Fee Related CN100412084C (zh) | 2003-07-02 | 2004-06-25 | 热稳定的结晶盐酸表柔比星及其制造方法 |
Country Status (7)
Country | Link |
---|---|
US (1) | US7485707B2 (zh) |
EP (1) | EP1638509B1 (zh) |
CN (1) | CN100412084C (zh) |
AT (1) | ATE520702T1 (zh) |
DE (1) | DE04777189T1 (zh) |
RU (1) | RU2341530C2 (zh) |
WO (1) | WO2005004805A2 (zh) |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102120750A (zh) * | 2011-01-30 | 2011-07-13 | 山东新时代药业有限公司 | 一种盐酸表柔比星的纯化方法 |
CN103827129A (zh) * | 2011-05-31 | 2014-05-28 | 贺利氏贵金属有限责任两合公司 | 盐酸表阿霉素的结晶 |
CN103906757A (zh) * | 2011-09-19 | 2014-07-02 | 贺利氏贵金属有限责任两合公司 | 盐酸伊达比星的结晶 |
CN104045672A (zh) * | 2013-03-15 | 2014-09-17 | 赛比亚斯药业有限公司 | 稳定的表柔比星盐酸盐结晶单水合物及其制备方法 |
CN104861014A (zh) * | 2015-06-03 | 2015-08-26 | 道中道(菏泽)制药有限公司 | 一种盐酸表阿霉素结晶的制备方法 |
Families Citing this family (17)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20090099346A1 (en) * | 2003-07-02 | 2009-04-16 | Victor Matvienko | Thermally stable crystalline epirubicin hydrochloride |
JP2008513519A (ja) * | 2005-05-11 | 2008-05-01 | シコール インコーポレイティド | 安定した凍結乾燥されたアントラサイクリングリコシド |
US8802830B2 (en) * | 2005-12-20 | 2014-08-12 | Solux Corporation | Synthesis of epirubicin from 13-dihydrodaunorubicine |
EP2636676A3 (en) * | 2009-09-08 | 2014-01-01 | Heraeus Precious Metals GmbH & Co. KG | Crystallization of epidaunorubicin x HCl |
KR101125460B1 (ko) * | 2010-03-24 | 2012-03-28 | 동아제약주식회사 | 에피루비신 염산염의 신규한 결정형 |
DK2582847T3 (en) | 2010-06-18 | 2016-12-19 | Myriad Genetics Inc | METHODS AND MATERIALS TO ASSESS loss of heterozygosity |
ES2588979T3 (es) | 2010-08-24 | 2016-11-08 | Dana-Farber Cancer Institute, Inc. | Procedimientos para la predicción de una respuesta contra el cáncer |
EP2721181B1 (en) | 2011-06-17 | 2019-12-18 | Myriad Genetics, Inc. | Methods and materials for assessing allelic imbalance |
DE102011111991A1 (de) * | 2011-08-30 | 2013-02-28 | Lead Discovery Center Gmbh | Neue Cyclosporin-Derivate |
JP6325453B2 (ja) | 2011-12-21 | 2018-05-16 | ミリアド・ジェネティックス・インコーポレイテッド | ヘテロ接合性の消失(lossofheterozygosity)を評価するための方法および材料 |
WO2013130347A1 (en) | 2012-02-23 | 2013-09-06 | The Children's Hospital Corporation | Methods for predicting anti-cancer response |
AU2013273466B2 (en) | 2012-06-07 | 2018-11-01 | Inserm (Institut National De La Sante Et De La Recherche Medicale) | Methods for detecting inactivation of the homologous recombination pathway (BRCA1/2) in human tumors |
US10308986B2 (en) | 2013-03-14 | 2019-06-04 | Children's Medical Center Corporation | Cancer diagnosis, treatment selection and treatment |
DK2981624T3 (da) | 2013-04-05 | 2020-03-02 | Myriad Genetics Inc | Fremgangsmåder til vurdering af homolog rekombinationsdeficiens og forudsigelse af respons på cancerbehandling |
EP3080292B1 (en) | 2013-12-09 | 2022-02-02 | Institut Curie | Methods for detecting inactivation of the homologous recombination pathway (brca1/2) in human tumors |
EP3180447B1 (en) | 2014-08-15 | 2020-03-11 | Myriad Genetics, Inc. | Methods and materials for assessing homologous recombination deficiency |
EP4141127A1 (en) | 2021-08-30 | 2023-03-01 | Zentrum Familiärer Brust- und Eierstockkrebs Universitätsklinik Köln | Method for assessing homologous recombination deficiency in ovarian cancer cells |
Family Cites Families (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB1506200A (en) * | 1975-04-30 | 1978-04-05 | Farmaceutici Italia | Glycosides |
US4345068A (en) * | 1979-11-22 | 1982-08-17 | Farmitalia Carlo Erba S.P.A. | Process for the preparation of 4'-epidaunorubicin, 3',4'-diepidaunorubicin, their doxorubicin analogs, and intermediates used in said process |
IT1155446B (it) * | 1982-12-23 | 1987-01-28 | Erba Farmitalia | Procedimento per la purificazione di glucosidi antraciclinonici mediante adsobimento selettivo su resine |
GB8426672D0 (en) * | 1984-10-22 | 1984-11-28 | Erba Farmitalia | Pharmaceutical compositions |
US5977082A (en) * | 1985-08-02 | 1999-11-02 | Pharmacia & Upjohn Company | Injectable ready-to-use solutions containing an antitumor anthracycline glycoside |
IT1275953B1 (it) * | 1995-03-22 | 1997-10-24 | Sicor Spa | Procedimento per la preparazione di antibiotici della classe delle antracicline |
PT848009E (pt) * | 1996-12-16 | 2000-11-30 | Pharmachemie Bv | Processo para a preparacao de epirubicina ou seus sais de adicao de acido a partir de daunorubicina |
WO1999028331A2 (en) * | 1997-11-28 | 1999-06-10 | Sumitomo Pharmaceuticals Co., Ltd. | Crystalline amrubicin hydrochloride |
-
2004
- 2004-06-25 WO PCT/US2004/020679 patent/WO2005004805A2/en active Application Filing
- 2004-06-25 DE DE04777189T patent/DE04777189T1/de active Pending
- 2004-06-25 AT AT04777189T patent/ATE520702T1/de not_active IP Right Cessation
- 2004-06-25 US US10/877,221 patent/US7485707B2/en active Active
- 2004-06-25 EP EP04777189.4A patent/EP1638509B1/en not_active Expired - Lifetime
- 2004-06-25 CN CNB2004800191272A patent/CN100412084C/zh not_active Expired - Fee Related
- 2004-06-25 RU RU2006101764/04A patent/RU2341530C2/ru not_active IP Right Cessation
Cited By (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102120750A (zh) * | 2011-01-30 | 2011-07-13 | 山东新时代药业有限公司 | 一种盐酸表柔比星的纯化方法 |
CN102120750B (zh) * | 2011-01-30 | 2013-04-03 | 山东新时代药业有限公司 | 一种盐酸表柔比星的纯化方法 |
CN103827129A (zh) * | 2011-05-31 | 2014-05-28 | 贺利氏贵金属有限责任两合公司 | 盐酸表阿霉素的结晶 |
TWI496789B (zh) * | 2011-05-31 | 2015-08-21 | Heraeus Precious Metals Gmbh | 表柔比星(epirubicin)鹽酸鹽之結晶 |
US9657047B2 (en) | 2011-05-31 | 2017-05-23 | Medac Gesellschaft für klinische Spezialpräparate mbH | Crystallization of epirubicin hydrochloride |
CN103906757A (zh) * | 2011-09-19 | 2014-07-02 | 贺利氏贵金属有限责任两合公司 | 盐酸伊达比星的结晶 |
CN104045672A (zh) * | 2013-03-15 | 2014-09-17 | 赛比亚斯药业有限公司 | 稳定的表柔比星盐酸盐结晶单水合物及其制备方法 |
CN104045672B (zh) * | 2013-03-15 | 2017-09-15 | 赛比亚斯药业股份公司 | 稳定的表柔比星盐酸盐结晶单水合物及其制备方法 |
CN104861014A (zh) * | 2015-06-03 | 2015-08-26 | 道中道(菏泽)制药有限公司 | 一种盐酸表阿霉素结晶的制备方法 |
Also Published As
Publication number | Publication date |
---|---|
CN100412084C (zh) | 2008-08-20 |
WO2005004805A3 (en) | 2006-06-22 |
RU2006101764A (ru) | 2007-08-10 |
US20060063726A1 (en) | 2006-03-23 |
DE04777189T1 (de) | 2011-04-07 |
EP1638509B1 (en) | 2015-12-30 |
WO2005004805A2 (en) | 2005-01-20 |
EP1638509A2 (en) | 2006-03-29 |
ATE520702T1 (de) | 2011-09-15 |
US7485707B2 (en) | 2009-02-03 |
EP1638509A4 (en) | 2009-12-09 |
RU2341530C2 (ru) | 2008-12-20 |
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C06 | Publication | ||
PB01 | Publication | ||
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SE01 | Entry into force of request for substantive examination | ||
C14 | Grant of patent or utility model | ||
GR01 | Patent grant | ||
C56 | Change in the name or address of the patentee | ||
CP01 | Change in the name or title of a patent holder |
Address after: American California Patentee after: Solux Corp. Address before: American California Patentee before: Solux Corp. |
|
C35 | Partial or whole invalidation of patent or utility model | ||
IP01 | Partial invalidation of patent right |
Commission number: 4W101242 Conclusion of examination: Claim No. 200480019127.2 and 7 of the invention are null and void and continue to maintain the patent on the basis of claim 1-2, 6 and 8-10 on the basis of claim 3-5. Decision date of declaring invalidation: 20120629 Decision number of declaring invalidation: 18902 Denomination of invention: Thermally stable crystalline epirubicin hydrochloride and method of making the same Granted publication date: 20080820 Patentee: Solux Corp. |
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CF01 | Termination of patent right due to non-payment of annual fee |