CN1976921A - (3r)-1-(2-甲基丙氨酰-d-色氨酰)-3-(苯甲基)-3-哌啶羧酸1,2,2-三甲基酰肼的晶形 - Google Patents
(3r)-1-(2-甲基丙氨酰-d-色氨酰)-3-(苯甲基)-3-哌啶羧酸1,2,2-三甲基酰肼的晶形 Download PDFInfo
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- CN1976921A CN1976921A CNA2005800215163A CN200580021516A CN1976921A CN 1976921 A CN1976921 A CN 1976921A CN A2005800215163 A CNA2005800215163 A CN A2005800215163A CN 200580021516 A CN200580021516 A CN 200580021516A CN 1976921 A CN1976921 A CN 1976921A
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- C07—ORGANIC CHEMISTRY
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- C07K5/00—Peptides containing up to four amino acids in a fully defined sequence; Derivatives thereof
- C07K5/02—Peptides containing up to four amino acids in a fully defined sequence; Derivatives thereof containing at least one abnormal peptide link
- C07K5/0202—Peptides containing up to four amino acids in a fully defined sequence; Derivatives thereof containing at least one abnormal peptide link containing the structure -NH-X-X-C(=0)-, X being an optionally substituted carbon atom or a heteroatom, e.g. beta-amino acids
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- A—HUMAN NECESSITIES
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- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/33—Heterocyclic compounds
- A61K31/395—Heterocyclic compounds having nitrogen as a ring hetero atom, e.g. guanethidine or rifamycins
- A61K31/435—Heterocyclic compounds having nitrogen as a ring hetero atom, e.g. guanethidine or rifamycins having six-membered rings with one nitrogen as the only ring hetero atom
- A61K31/44—Non condensed pyridines; Hydrogenated derivatives thereof
- A61K31/445—Non condensed piperidines, e.g. piperocaine
- A61K31/4523—Non condensed piperidines, e.g. piperocaine containing further heterocyclic ring systems
- A61K31/454—Non condensed piperidines, e.g. piperocaine containing further heterocyclic ring systems containing a five-membered ring with nitrogen as a ring hetero atom, e.g. pimozide, domperidone
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- C07D401/02—Heterocyclic compounds containing two or more hetero rings, having nitrogen atoms as the only ring hetero atoms, at least one ring being a six-membered ring with only one nitrogen atom containing two hetero rings
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Abstract
Description
峰 | 2θ | d | 相对强度 |
No. | (度) | (A) | |
1 | 2.6 | 33.7 | 3 |
2 | 2.9 | 30.6 | 4 |
3 | 4.0 | 22.34 | 3 |
4 | 4.7 | 18.8 | 3 |
5 | 7.1 | 12.4 | 3 |
6 | 9.3 | 9.5 | 8 |
7 | 16.1 | 5.5 | 4 |
8 | 16.6 | 5.3 | 4 |
9 | 17.0 | 5.2 | 100 |
10 | 17.6 | 5.0 | 6 |
11 | 19.4 | 4.6 | 9 |
12 | 20.1 | 4.4 | 3 |
13 | 20.4 | 4.4 | 8 |
14 | 20.6 | 4.3 | 4 |
15 | 21.5 | 4.1 | 10 |
16 | 22.9 | 3.9 | 7 |
17 | 23.1 | 3.9 | 6 |
18 | 23.3 | 3.8 | 6 |
19 | 23.5 | 3.8 | 9 |
20 | 24.1 | 3.7 | 4 |
21 | 25.4 | 3.5 | 4 |
22 | 26.2 | 3.4 | 37 |
23 | 26.5 | 3.4 | 4 |
24 | 27.1 | 3.3 | 6 |
25 | 27.4 | 3.3 | 5 |
26 | 29.8 | 3.0 | 6 |
27 | 30.0 | 3.0 | 4 |
28 | 30.7 | 2.9 | 4 |
29 | 30.9 | 2.9 | 3 |
30 | 31.5 | 2.8 | 5 |
31 | 33.3 | 2.7 | 18 |
32 | 34.7 | 2.6 | 4 |
33 | 35.1 | 2.6 | 3 |
34 | 37.2 | 2.4 | 4 |
35 | 37.3 | 2.4 | 5 |
36 | 37.5 | 2.4 | 4 |
37 | 37.9 | 2.4 | 3 |
38 | 38.1 | 2.4 | 3 |
39 | 38.4 | 2.3 | 4 |
40 | 38.8 | 2.3 | 4 |
峰 | 2θ | D | 相对强度 |
No. | (度) | (A) | |
1 | 8.1 | 10.9 | 8 |
2 | 9.0 | 9.8 | 4 |
3 | 9.6 | 9.2 | 8 |
4 | 10.7 | 8.3 | 4 |
5 | 13.6 | 6.5 | 8 |
6 | 14.3 | 6.2 | 12 |
7 | 16.3 | 5.4 | 40 |
8 | 17.5 | 5.1 | 12 |
9 | 18.0 | 4.9 | 12 |
10 | 19.2 | 4.6 | 68 |
11 | 20.1 | 4.4 | 56 |
12 | 21.4 | 4.2 | 20 |
13 | 23.0 | 3.9 | 100 |
14 | 24.0 | 3.7 | 16 |
15 | 24.6 | 3.6 | 4 |
16 | 25.3 | 3.5 | 12 |
17 | 26.2 | 3.4 | 100 |
18 | 27.0 | 3.3 | 52 |
19 | 29.8 | 3.0 | 16 |
20 | 31.5 | 2.8 | 32 |
21 | 33.1 | 2.7 | 16 |
22 | 34.1 | 2.6 | 12 |
23 | 35.3 | 2.5 | 8 |
24 | 37.4 | 2.4 | 4 |
25 | 38.6 | 2.3 | 8 |
峰 | 2θ | d | 相对强度 |
No. | (度) | (A) | |
1 | 9.4 | 9.4 | 3 |
2 | 9.9 | 9.0 | 24 |
3 | 10.2 | 8.7 | 76 |
4 | 10.6 | 8.3 | 15 |
5 | 11.2 | 7.9 | 55 |
6 | 11.7 | 7.6 | 8 |
7 | 13.8 | 6.4 | 24 |
8 | 14.3 | 6.2 | 43 |
9 | 14.6 | 6.1 | 9 |
10 | 15.1 | 5.9 | 24 |
11 | 16.7 | 5.3 | 24 |
12 | 17.4 | 5.1 | 18 |
13 | 17.9 | 5.0 | 23 |
14 | 18.2 | 4.9 | 15 |
15 | 18.7 | 4.7 | 53 |
16 | 19.8 | 4.5 | 40 |
17 | 20.6 | 4.3 | 100 |
18 | 21.1 | 4.2 | 5 |
19 | 21.6 | 4.1 | 9 |
20 | 21.8 | 4.1 | 10 |
21 | 22.5 | 4.0 | 7 |
22 | 23.4 | 3.8 | 56 |
23 | 23.8 | 3.7 | 6 |
24 | 24.9 | 3.6 | 9 |
25 | 25.8 | 3.5 | 13 |
26 | 26.4 | 3.4 | 6 |
27 | 27.5 | 3.2 | 11 |
28 | 27.7 | 3.2 | 21 |
29 | 28.8 | 3.1 | 13 |
30 | 30.0 | 3.0 | 14 |
31 | 30.4 | 3.0 | 18 |
32 | 31.3 | 2.9 | 13 |
33 | 31.9 | 2.8 | 6 |
34 | 32.9 | 2.7 | 4 |
35 | 33.6 | 2.7 | 18 |
36 | 34.1 | 2.6 | 9 |
37 | 34.4 | 2.6 | 4 |
38 | 35.5 | 2.5 | 7 |
39 | 36.8 | 2.4 | 10 |
40 | 37.4 | 2.4 | 11 |
峰 | 2θ | d | 相对强度 |
No. | (度) | (A) | |
1 | 9.6 | 9.2 | 8 |
2 | 10.1 | 8.8 | 100 |
3 | 10.8 | 8.2 | 4 |
4 | 11.1 | 8.0 | 25 |
5 | 13.8 | 6.4 | 7 |
6 | 14.6 | 6.1 | 4 |
7 | 15.2 | 5.8 | 6 |
8 | 16.7 | 5.3 | 6 |
9 | 17.3 | 5.1 | 9 |
10 | 17.6 | 5.0 | 18 |
11 | 18.2 | 4.9 | 12 |
12 | 20.0 | 4.4 | 18 |
13 | 20.5 | 4.3 | 7 |
14 | 20.8 | 4.3 | 12 |
15 | 22.1 | 4.0 | 8 |
16 | 23.5 | 3.8 | 13 |
17 | 25.8 | 3.5 | 4 |
18 | 27.5 | 3.2 | 5 |
19 | 30.5 | 3.0 | 4 |
20 | 35.0 | 2.6 | 3 |
试验(试验方法) | 说明 | 贮存条件 | 间隔(月) | ||||||||
起始 | 1 | 3 | 6 | 9 | 12 | 18 | 24 | 36 | |||
物理描述(TM·106) | 白色到近白色固体 | 5℃25℃/60%RH30℃/60%RH40℃/75%RH | 近白色固体 | 近白色固体近白色固体-近白色固体 | 近白色固体近白色固体-近白色固体 | 近白色固体近白色固体-近白色固体 | 白色固体近白色固体-- | 近白色固体近白色固体-- | |||
通过卡尔-费歇尔法测的水含量(USP<921>,方法1dSOP(NS002) | 仅供参考 | 5℃25℃/60%RH30℃/60%RH40℃/75%RH | 3.2% | 5.3%5.8%-6.1% | 6.0%6.0%-6.1% | 5.8%5.9%-5.9% | 5.6%5.7%-- | 6.1%5.8%-- | |||
HPLC重量%(TM·808) | 仅供参考 | 5℃25℃/60%RH3O℃/60%RH40℃/75%RH | 99.8% | 92.0%92.1%-91.8% | 93.2%93.2%-93.0% | 93.9%94.2%-94.1% | 94.5%94.6%-- | 94.3%94.2%-- | |||
HPLC面积%(TM·808)1 | 不少于98% | 5℃25℃/60%RH30℃/60%RH40℃/75%RH | 99.8% | 99.7%99.7%-99.7% | 99.7%99.7%-99.7% | 99.7%99.7%-99.7% | 99.8%99.8%-- | 99.7%99.7%-- | |||
DSC(USP<891>,SOP(NS034) | 仅供参考 | 5℃25℃/60%RH30℃/60%RH40℃/75%RH | 起始:108.2℃峰:112.7℃ | 起始:81.8℃峰:110.4℃起始:116.0℃峰:118.4℃起始:107.0℃峰:1103℃起始:121.3℃峰:122.2℃-起始:89.2℃峰:110.3℃起始:129.9℃峰:134.9℃起始:157.1℃峰:18.2℃ | 起始:112.1℃峰:117.1℃起始:112.6℃峰:117.7℃-起始:112.2℃峰:117.5℃ | 起始:112.3℃峰:116.9℃起始:112.5℃峰:116.9℃-起始:112.6℃峰:11.6℃ | ---- | ---- | |||
使用光学显微镜观察的结晶性(USP<695>) | 仅供参考 | 5℃25℃/60%RH30℃/60%RH40℃/75%RH | 结晶 | 结晶结晶-结晶 | 结晶结晶-结晶 | 结晶结晶-结晶 | 结晶结晶-- | 结晶结晶-- |
Claims (67)
Priority Applications (1)
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CN201110251236.9A CN102584937B (zh) | 2004-06-29 | 2005-06-22 | (3r)‑1‑(2‑甲基丙氨酰‑d‑色氨酰)‑3‑(苯甲基)‑3‑哌啶羧酸1,2,2‑三甲基酰肼的晶形 |
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Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US58375704P | 2004-06-29 | 2004-06-29 | |
US60/583,757 | 2004-06-29 | ||
PCT/US2005/022408 WO2006016995A1 (en) | 2004-06-29 | 2005-06-22 | Crystal forms of (3r)-1-(2-methylalanyl-d-tryptophyl)-3-(phenylmethyl)-3-piperidinecarboxylic acid 1,2,2-trimethylhydrazide |
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CN201110251236.9A Division CN102584937B (zh) | 2004-06-29 | 2005-06-22 | (3r)‑1‑(2‑甲基丙氨酰‑d‑色氨酰)‑3‑(苯甲基)‑3‑哌啶羧酸1,2,2‑三甲基酰肼的晶形 |
CN201310308801.XA Division CN103772483A (zh) | 2004-06-29 | 2005-06-22 | (3r)-1-(2-甲基丙氨酰-d-色氨酰)-3-(苯甲基)-3-哌啶羧酸1,2,2-三甲基酰肼的晶形 |
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CN1976921A true CN1976921A (zh) | 2007-06-06 |
CN1976921B CN1976921B (zh) | 2013-08-21 |
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CN2005800215163A Active CN1976921B (zh) | 2004-06-29 | 2005-06-22 | (3r)-1-(2-甲基丙氨酰-d-色氨酰)-3-(苯甲基)-3-哌啶羧酸1,2,2-三甲基酰肼的晶形 |
CN201310308801.XA Pending CN103772483A (zh) | 2004-06-29 | 2005-06-22 | (3r)-1-(2-甲基丙氨酰-d-色氨酰)-3-(苯甲基)-3-哌啶羧酸1,2,2-三甲基酰肼的晶形 |
CN201110251236.9A Active CN102584937B (zh) | 2004-06-29 | 2005-06-22 | (3r)‑1‑(2‑甲基丙氨酰‑d‑色氨酰)‑3‑(苯甲基)‑3‑哌啶羧酸1,2,2‑三甲基酰肼的晶形 |
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CN201310308801.XA Pending CN103772483A (zh) | 2004-06-29 | 2005-06-22 | (3r)-1-(2-甲基丙氨酰-d-色氨酰)-3-(苯甲基)-3-哌啶羧酸1,2,2-三甲基酰肼的晶形 |
CN201110251236.9A Active CN102584937B (zh) | 2004-06-29 | 2005-06-22 | (3r)‑1‑(2‑甲基丙氨酰‑d‑色氨酰)‑3‑(苯甲基)‑3‑哌啶羧酸1,2,2‑三甲基酰肼的晶形 |
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US (2) | US7825138B2 (zh) |
EP (2) | EP1768976B1 (zh) |
JP (2) | JP5122950B2 (zh) |
KR (1) | KR101324340B1 (zh) |
CN (3) | CN1976921B (zh) |
CA (1) | CA2572325C (zh) |
HK (1) | HK1105000A1 (zh) |
IL (1) | IL180336A0 (zh) |
MX (1) | MXPA06015003A (zh) |
WO (1) | WO2006016995A1 (zh) |
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US7825138B2 (en) * | 2004-06-29 | 2010-11-02 | Helsinn Therapeutics (U.S.), Inc. | Crystal forms of (3R)-1-(2-methylalanyl-D-tryptophyl)-3-(phenylmethyl)-3-piperidinecarboxylic acid 1,2,2-trimethylhydrazide |
US20130281701A1 (en) | 2004-06-29 | 2013-10-24 | Helsinn Therapeutics (U.S.), Inc. | Crystal forms of anamorelin |
JO3353B1 (ar) | 2012-04-20 | 2019-03-13 | Ono Pharmaceutical Co | شكل صلب معزول من أحادي هيدروكلوريد أناموريلين بنسبة مولارية منخفضة من الكلوريد: أناموريلين ومحتوى منخفض من مذيب عضوي متبقي |
MX363715B (es) * | 2013-02-21 | 2019-03-29 | Pfizer | Formas solidas de un inhbidor de cdk4/6 selectivo. |
WO2016036598A1 (en) | 2014-09-04 | 2016-03-10 | Helsinn Healthcare Sa | Medical treatments based on anamorelin |
CN107001323A (zh) * | 2015-10-20 | 2017-08-01 | 江苏恒瑞医药股份有限公司 | 一种阿拉莫林的结晶形式及其制备方法 |
US9837965B1 (en) | 2016-09-16 | 2017-12-05 | Peregrine Semiconductor Corporation | Standby voltage condition for fast RF amplifier bias recovery |
WO2021038519A1 (en) | 2019-08-30 | 2021-03-04 | Helsinn Healthcare Sa | Methods of manufacturing anamorelin tablets having improved stability |
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SK56296A3 (en) * | 1993-11-09 | 1997-02-05 | Merck & Co Inc | Piperidinal, pyrrolidinal and hexahydro-1h-azepinal derivatives, manufacturing process thereof and pharmaceutical compositions containing them |
DE69713109T2 (de) * | 1996-07-22 | 2003-01-02 | Novo Nordisk A/S, Bagsvaerd | Verbindungen mit wachstumshormon freisetzenden eigenschaften |
EP1047709B1 (en) * | 1998-01-16 | 2004-11-03 | Novo Nordisk A/S | Compounds with growth hormone releasing properties |
US6303620B1 (en) | 1998-05-11 | 2001-10-16 | Novo Nordisk A/S | Compounds with growth hormone releasing properties |
JP4142253B2 (ja) * | 1998-05-11 | 2008-09-03 | ノボ ノルディスク アクティーゼルスカブ | 成長ホルモン放出特性を有する化合物 |
ID29137A (id) * | 1998-07-27 | 2001-08-02 | Schering Corp | Ligan-ligan afinitas tinggi untuk reseptor nosiseptin orl-1 |
UA73530C2 (uk) * | 1999-11-10 | 2005-08-15 | Ново Нордіск А/С | Сполука з властивостями вивільнювати гормон росту |
CA2565324A1 (en) * | 2004-03-30 | 2005-10-20 | Sapphire Therapeutics, Inc. | Method of reducing c-reactive protein using growth hormone secretagogues |
US7825138B2 (en) | 2004-06-29 | 2010-11-02 | Helsinn Therapeutics (U.S.), Inc. | Crystal forms of (3R)-1-(2-methylalanyl-D-tryptophyl)-3-(phenylmethyl)-3-piperidinecarboxylic acid 1,2,2-trimethylhydrazide |
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- 2005-06-22 CN CN2005800215163A patent/CN1976921B/zh active Active
- 2005-06-22 JP JP2007519301A patent/JP5122950B2/ja active Active
- 2005-06-22 CN CN201310308801.XA patent/CN103772483A/zh active Pending
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Also Published As
Publication number | Publication date |
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JP5122950B2 (ja) | 2013-01-16 |
HK1105000A1 (zh) | 2008-02-01 |
JP2012188452A (ja) | 2012-10-04 |
KR101324340B1 (ko) | 2013-10-31 |
US20110003996A1 (en) | 2011-01-06 |
US20070004638A1 (en) | 2007-01-04 |
MXPA06015003A (es) | 2007-08-07 |
IL180336A0 (en) | 2007-07-04 |
JP2008505078A (ja) | 2008-02-21 |
CN102584937B (zh) | 2017-03-01 |
US7825138B2 (en) | 2010-11-02 |
EP1768976A1 (en) | 2007-04-04 |
CN1976921B (zh) | 2013-08-21 |
US8466173B2 (en) | 2013-06-18 |
KR20070030222A (ko) | 2007-03-15 |
EP2298760A1 (en) | 2011-03-23 |
CA2572325A1 (en) | 2006-02-16 |
CN103772483A (zh) | 2014-05-07 |
CN102584937A (zh) | 2012-07-18 |
CA2572325C (en) | 2013-08-27 |
EP1768976B1 (en) | 2017-04-26 |
JP5718286B2 (ja) | 2015-05-13 |
EP2298760B1 (en) | 2015-08-05 |
WO2006016995A1 (en) | 2006-02-16 |
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