CN104788438A - 恩格列净b晶型及其制备 - Google Patents
恩格列净b晶型及其制备 Download PDFInfo
- Publication number
- CN104788438A CN104788438A CN201510160852.1A CN201510160852A CN104788438A CN 104788438 A CN104788438 A CN 104788438A CN 201510160852 A CN201510160852 A CN 201510160852A CN 104788438 A CN104788438 A CN 104788438A
- Authority
- CN
- China
- Prior art keywords
- gelie
- crystal form
- clean
- degree
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- LYOVGHSJHHIGMP-JKTNAWMUSA-N OCC(CC(CO)O[C@H]1c(cc2)cc(Cc(cc3)ccc3OC3COCC3)c2Cl)[C@H]1O Chemical compound OCC(CC(CO)O[C@H]1c(cc2)cc(Cc(cc3)ccc3OC3COCC3)c2Cl)[C@H]1O LYOVGHSJHHIGMP-JKTNAWMUSA-N 0.000 description 1
- LZZUHMWPQYXTJY-VFMKGFAKSA-N OC[C@H]([C@H]([C@@H](C1)O)O)O[C@H]1c(cc1Cc(cc2)ccc2O[C@@H]2COCC2)ccc1Cl Chemical compound OC[C@H]([C@H]([C@@H](C1)O)O)O[C@H]1c(cc1Cc(cc2)ccc2O[C@@H]2COCC2)ccc1Cl LZZUHMWPQYXTJY-VFMKGFAKSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D407/00—Heterocyclic compounds containing two or more hetero rings, at least one ring having oxygen atoms as the only ring hetero atoms, not provided for by group C07D405/00
- C07D407/02—Heterocyclic compounds containing two or more hetero rings, at least one ring having oxygen atoms as the only ring hetero atoms, not provided for by group C07D405/00 containing two hetero rings
- C07D407/12—Heterocyclic compounds containing two or more hetero rings, at least one ring having oxygen atoms as the only ring hetero atoms, not provided for by group C07D405/00 containing two hetero rings linked by a chain containing hetero atoms as chain links
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07B—GENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
- C07B2200/00—Indexing scheme relating to specific properties of organic compounds
- C07B2200/13—Crystalline forms, e.g. polymorphs
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
Description
处方 | 组份 | 10mg片剂 | 25mg片剂 |
(1) | 恩格列净B晶型原料药 | 10mg | 25mg |
(2) | 乳糖 | 100mg | 90mg |
(3) | 微晶纤维素 | 45mg | 25mg |
(4) | 交联羧甲基纤维素钠 | 5mg | 5mg |
(5) | 5%聚维酮水溶液 | 50mg | 40mg |
(6) | 二氧化硅 | 1mg | 1mg |
(7) | 硬脂酸镁 | 1mg | 1mg |
NO. | 步骤 |
1 | 称取适量的(1)、(2)、(3)、(4)加入到高剪切的湿法制粒机中,干混1分钟; |
2 | 向上述制粒机中加入合适量的(5)制成颗粒; |
3 | 将颗粒置于流化床干燥器中干燥; |
4 | 干燥颗粒过筛; |
5 | 过筛后的颗粒与(6)和(7)置于混合器中混合5分钟; |
6 | 将混合好的物料,通过压片机压制成目标重量的片剂。 |
片剂10mg | 水 | pH6.8 | 0.1N盐酸 | pH4.5 |
5 | 84.9% | 88.7% | 83.3% | 86.5% |
10 | 94.8% | 97.6% | 92.7% | 97.4% |
15 | 95.5% | 98.2% | 93.2% | 98.3% |
30 | 98.6% | 98.0% | 97.1% | 98.7% |
45 | 98.5% | 98.1% | 98.4% | 98.7% |
JARDIANCE-10mg | 水 | pH6.8 | 0.1N盐酸 | pH4.5 |
5 | 71.8% | 77.3% | 75.3% | 74.8% |
10 | 91.4% | 92.7% | 90.4% | 91.3% |
15 | 93.9% | 96.4% | 91.9% | 93.4% |
30 | 93.2% | 96.9% | 92.6% | 94.4% |
45 | 93.0% | 96.5% | 92.4% | 94.8% |
片剂25mg | 水 | pH6.8 | 0.1N盐酸 | pH4.5 |
5 | 89.2% | 92.5% | 85.5% | 90.2% |
10 | 95.0% | 98.2% | 95.2% | 95.7% |
15 | 96.7% | 98.5% | 98.1% | 96.1% |
30 | 97.8% | 98.6% | 98.9% | 98.9% |
45 | 98.7% | 99.6% | 99.6% | 99.5% |
JARDIANCE-25mg | 水 | pH6.8 | 0.1N盐酸 | pH4.5 |
5 | 76.7% | 71.1% | 71.1% | 74.3% |
10 | 90.5% | 93.3% | 91.3% | 90.7% |
15 | 93.0% | 94.2% | 93.6% | 91.5% |
30 | 94.0% | 95.8% | 94.4% | 92.9% |
45 | 94.0% | 95.8% | 95.4% | 93.8% |
0天 | 总杂% |
自研片剂10mg | 0.13 |
JARDIANCE10mg | 0.19 |
自研片剂25mg | 0.13 |
JARDIANCE25mg | 0.19 |
10天 | 总杂% |
自研片剂10mg-60℃ | 0.14 |
自研片剂10mg-RH92.5% | 0.14 |
自研片剂10mg-4500lx±500 | 0.15 |
JARDIANCE10mg-60℃ | 0.28 |
JARDIANCE10mg-RH92.5% | 0.25 |
JARDIANCE10mg-4500lx±500 | 0.38 |
自研片剂25mg-60℃ | 0.17 |
自研片剂25mg-RH92.5% | 0.16 |
自研片剂25mg-4500lx±500 | 0.20 |
JARDIANCE25mg-60℃ | 0.31 |
JARDIANCE25mg-RH92.5% | 0.29 |
JARDIANCE25mg-4500lx±500 | 0.43 |
Claims (5)
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201510160852.1A CN104788438B (zh) | 2015-05-04 | 2015-05-04 | 恩格列净b晶型及其制备 |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201510160852.1A CN104788438B (zh) | 2015-05-04 | 2015-05-04 | 恩格列净b晶型及其制备 |
Publications (2)
Publication Number | Publication Date |
---|---|
CN104788438A true CN104788438A (zh) | 2015-07-22 |
CN104788438B CN104788438B (zh) | 2018-02-02 |
Family
ID=53553675
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201510160852.1A Active CN104788438B (zh) | 2015-05-04 | 2015-05-04 | 恩格列净b晶型及其制备 |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN104788438B (zh) |
Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105399735A (zh) * | 2015-12-29 | 2016-03-16 | 上海应用技术学院 | 一种艾格列净中间体及其制备方法和应用 |
CN106336403A (zh) * | 2015-07-14 | 2017-01-18 | 江苏豪森药业集团有限公司 | 依帕列净的工业制备方法 |
CN106706768A (zh) * | 2015-11-17 | 2017-05-24 | 重庆医药工业研究院有限责任公司 | 一种分离测定恩格列净及其有关物质的方法 |
WO2017130217A1 (en) * | 2016-01-27 | 2017-08-03 | Msn Laboratories Private Limited | The present invention relates to process for the preparation of d-glucitol, 1,5- anhydro-1-c-[4-chloro-3-[[4-[[(3s)-tetrahydro-3-furanyl] oxy]phenyl] methyl]phenyl]-, (1s) and its crystalline forms thereof. |
CN108794548A (zh) * | 2017-04-28 | 2018-11-13 | 正大天晴药业集团股份有限公司 | 制备恩格列净及其中间体的方法 |
CN111983054A (zh) * | 2020-07-28 | 2020-11-24 | 安徽联创生物医药股份有限公司 | 一种用hplc分离测定依帕列净中间体有关物质的方法 |
CN116063294A (zh) * | 2022-12-13 | 2023-05-05 | 山东能源集团新材料有限公司 | 一种恩格列净原料药的制备方法及工艺*** |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2002083066A2 (en) * | 2001-04-11 | 2002-10-24 | Bristol-Myers Squibb Company | Amino acid complexes of c-aryl glucosides for treatment of diabetes and method |
CN101155794A (zh) * | 2005-05-03 | 2008-04-02 | 贝林格尔·英格海姆国际有限公司 | 1-氯-4-(β-D-吡喃葡萄糖-1-基)-2-[4-((S)-四氢呋喃-3-基氧基)-苄基]-苯的晶型、其制备方法及其用于制备药物的用途 |
CN101193903A (zh) * | 2005-05-10 | 2008-06-04 | 贝林格尔.英格海姆国际有限公司 | 制备吡喃葡萄糖基取代的苄基苯衍生物及其中间体的方法 |
CN102549005A (zh) * | 2009-09-30 | 2012-07-04 | 贝林格尔.英格海姆国际有限公司 | 1-氯-4-(β-D-吡喃葡萄糖-1-基)-2-[4-((S)-四氢呋喃-3-基氧基)-苄基]-苯的晶型的制备方法 |
-
2015
- 2015-05-04 CN CN201510160852.1A patent/CN104788438B/zh active Active
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2002083066A2 (en) * | 2001-04-11 | 2002-10-24 | Bristol-Myers Squibb Company | Amino acid complexes of c-aryl glucosides for treatment of diabetes and method |
CN101155794A (zh) * | 2005-05-03 | 2008-04-02 | 贝林格尔·英格海姆国际有限公司 | 1-氯-4-(β-D-吡喃葡萄糖-1-基)-2-[4-((S)-四氢呋喃-3-基氧基)-苄基]-苯的晶型、其制备方法及其用于制备药物的用途 |
CN101193903A (zh) * | 2005-05-10 | 2008-06-04 | 贝林格尔.英格海姆国际有限公司 | 制备吡喃葡萄糖基取代的苄基苯衍生物及其中间体的方法 |
CN102549005A (zh) * | 2009-09-30 | 2012-07-04 | 贝林格尔.英格海姆国际有限公司 | 1-氯-4-(β-D-吡喃葡萄糖-1-基)-2-[4-((S)-四氢呋喃-3-基氧基)-苄基]-苯的晶型的制备方法 |
Cited By (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106336403A (zh) * | 2015-07-14 | 2017-01-18 | 江苏豪森药业集团有限公司 | 依帕列净的工业制备方法 |
CN106706768A (zh) * | 2015-11-17 | 2017-05-24 | 重庆医药工业研究院有限责任公司 | 一种分离测定恩格列净及其有关物质的方法 |
CN105399735A (zh) * | 2015-12-29 | 2016-03-16 | 上海应用技术学院 | 一种艾格列净中间体及其制备方法和应用 |
WO2017130217A1 (en) * | 2016-01-27 | 2017-08-03 | Msn Laboratories Private Limited | The present invention relates to process for the preparation of d-glucitol, 1,5- anhydro-1-c-[4-chloro-3-[[4-[[(3s)-tetrahydro-3-furanyl] oxy]phenyl] methyl]phenyl]-, (1s) and its crystalline forms thereof. |
US10913762B2 (en) | 2016-01-27 | 2021-02-09 | Msn Laboratories Private Limited | Process for the preparation of D-glucitol, 1,5-anhydro-1-C-[4-chloro-3-[[4-[[(3S)-tetrahydro-3-furanyl] oxy]phenyl] methyl] phenyl]-, (1S) and its crystalline forms thereof |
CN108794548A (zh) * | 2017-04-28 | 2018-11-13 | 正大天晴药业集团股份有限公司 | 制备恩格列净及其中间体的方法 |
CN108794548B (zh) * | 2017-04-28 | 2023-06-16 | 正大天晴药业集团股份有限公司 | 制备恩格列净及其中间体的方法 |
CN111983054A (zh) * | 2020-07-28 | 2020-11-24 | 安徽联创生物医药股份有限公司 | 一种用hplc分离测定依帕列净中间体有关物质的方法 |
CN116063294A (zh) * | 2022-12-13 | 2023-05-05 | 山东能源集团新材料有限公司 | 一种恩格列净原料药的制备方法及工艺*** |
Also Published As
Publication number | Publication date |
---|---|
CN104788438B (zh) | 2018-02-02 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN104788438A (zh) | 恩格列净b晶型及其制备 | |
CN105120844A (zh) | 杂环化合物和其用途 | |
CN105367515B (zh) | 一种氢溴酸沃替西汀α晶型的制备方法 | |
KR20120113285A (ko) | 다사티닙 다결정체 및 그의 제조방법과 약물 조성물 | |
CN110483486B (zh) | 一种奥西替尼酮咯酸盐晶型及其制备方法 | |
CN102827153B (zh) | 阿齐沙坦的晶型及其制备方法 | |
AU2013330603B2 (en) | Monohydrate crystal of fimasartan potassium salt, method for preparing same, and pharmacological composition comprising same | |
CN104592195A (zh) | 一种苯甲酸阿格列汀的制备方法 | |
AU2016269359B2 (en) | Sodium salt of uric acid transporter inhibitor and crystalline form thereof | |
CN103880829B (zh) | 一种阿齐沙坦晶体及其制备方法和用途 | |
CN104721828A (zh) | 一种改善晶体药物稳定性的药物组合物及其制备方法 | |
CN105439980B (zh) | 一种氢溴酸沃替西汀一仲丁醇合物及其制备方法 | |
CN104817557B (zh) | 一种盐酸莫西沙星的稳定晶型及其制备方法 | |
CN102070558B (zh) | 非布索坦的新晶型及其制备方法 | |
US20070032506A1 (en) | Crystalline forms of (2r-trans)-6-chloro-5[[4-[(4-fluorophenyl)methyl]-2,5-dimethyl-1-piperazinyl]carbonyl]-n,n, 1-trimethyl-alpha-oxo-1h-indole-3-acetamide monohydrochloride | |
CN104725377B (zh) | 一种盐酸莫西沙星的晶型及其制备方法 | |
CN104829483B (zh) | 一种盐酸丙帕他莫a晶型的制备方法 | |
CN105153066B (zh) | 盐酸沃替西汀的结晶型物及其制备方法 | |
CN105037341B (zh) | 阿齐沙坦醇铵晶型及其制备方法 | |
CN104130245A (zh) | 盐酸帕唑帕尼n晶型及其制备 | |
CN103588653B (zh) | 4-甲基苯甲酸4-[2-二甲基胺基-1-(1-羟基环己基)乙基]苯酯盐酸盐的多晶型物、制备方法及其应用 | |
CN107954947A (zh) | 沃替西汀氢溴酸盐晶型c及其制备方法 | |
CN104693200B (zh) | 一种盐酸莫西沙星的晶型及其制备方法 | |
CN105399742A (zh) | 那格列汀a晶型及药物组合物 | |
CN105461618A (zh) | 甲磺酸洛美他派新晶型及其制备方法 |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
C06 | Publication | ||
PB01 | Publication | ||
EXSB | Decision made by sipo to initiate substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
CB02 | Change of applicant information |
Address after: Cheng Wei Road Nanjing city Jiangsu province 210012 Xianlin University No. 9 Applicant after: Nanjing Huawei Medicine Technology Group Co Ltd Address before: Cheng Wei Road Nanjing city Jiangsu province 210012 Xianlin University No. 9 Applicant before: Nanjing Huawe Medical Science & Technology Development Co., Ltd. |
|
CB02 | Change of applicant information | ||
GR01 | Patent grant | ||
GR01 | Patent grant | ||
TR01 | Transfer of patent right |
Effective date of registration: 20191204 Address after: Building F2, No.9, Weidi Road, Qixia District, Nanjing City, Jiangsu Province Patentee after: Jiangsu Li Hua Bioisystech Co., Ltd Address before: Cheng Wei Road Nanjing city Jiangsu province 210012 Xianlin University No. 9 Patentee before: Nanjing Huawei Medicine Technology Group Co Ltd |
|
TR01 | Transfer of patent right |