CN105636964A - L-丙氨酸-(14-冬凌草甲素)酯三氟乙酸盐的i型结晶及制备方法 - Google Patents
L-丙氨酸-(14-冬凌草甲素)酯三氟乙酸盐的i型结晶及制备方法 Download PDFInfo
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- CN105636964A CN105636964A CN201580002233.8A CN201580002233A CN105636964A CN 105636964 A CN105636964 A CN 105636964A CN 201580002233 A CN201580002233 A CN 201580002233A CN 105636964 A CN105636964 A CN 105636964A
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/33—Heterocyclic compounds
- A61K31/335—Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin
- A61K31/35—Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin having six-membered rings with one oxygen as the only ring hetero atom
- A61K31/352—Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin having six-membered rings with one oxygen as the only ring hetero atom condensed with carbocyclic rings, e.g. methantheline
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- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D493/00—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system
- C07D493/02—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system in which the condensed system contains two hetero rings
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Abstract
Description
Claims (7)
- 一种L-丙氨酸-(14-冬凌草甲素)酯三氟乙酸盐的I型结晶,其特征在于使用Cu-Ka辐射,得到以2θ角度和晶面间距表示的X-射线粉末衍射图谱,所述结晶具有如图1所示的X-射线粉末衍射图谱,其中在约6.85(12.89),8.09(10.92),11.30(7.82),13.71(6.45),14.08(6.29),14.35(6.17),16.40(5.40),17.41(5.09),18.19(4.87),18.44(4.81),20.12(4.41),21.17(4.19),23.38(3.80),23.88(3.72),24.42(3.64),24.84(3.58),25.72(3.46),26.46(3.37),27.22(3.27),28.40(3.14),29.38(3.04),31.26(2.86)和31.79(2.81)有特征峰。
- 一种制备如权利要求1所述的L-丙氨酸-(14-冬凌草甲素)酯三氟乙酸盐的I型结晶的方法,所述方法包括下述步骤:1)将任意晶型或无定型的N-Boc-L-丙氨酸-(14-冬凌草甲素)酯与三氟乙酸,或者任意晶型或无定型的L-丙氨酸-(14-冬凌草甲素)酯三氟乙酸盐固体常温溶解于有机溶剂中,搅拌析晶,或加入反溶剂后,搅拌析晶,所述有机溶剂选自碳原子数小于等于3的醇类、卤代烃、酮类、酯类中的一种或几种,或者为选自碳原子数小于等于3的醇类、卤代烃、酮类、酯类中的任意一种或几种与碳原子数小于等于3的醚类的混合溶剂;优选所述的有机溶剂选自酮类、醇类、酯类的一种或几种,或者为选自酮类、醇类、酯类中的任意一种或几种与醚类的混合溶剂;2)过滤结晶并洗涤,干燥。
- 根据权利要求2所述的方法,其特征在于在步骤1)中所述的有机溶剂为丙酮、乙酸乙酯、二氯甲烷/乙醚、丙酮/异丙醚、二氯甲烷/异丙醚、乙醇/异丙醚、异丙醇/异丙醚、甲醇/异丙醚。
- 根据权利要求3所述的方法,其步骤1)中所述的有机溶剂为丙酮/异丙醚。
- 一种药物组合物,其含有如权利要求1所述的L-丙氨酸-(14-草甲素)酯三氟乙酸盐的I型结晶以及药学上可接受的载体。
- 根据权利要求1所述的L-丙氨酸-(14-草甲素)酯三氟乙酸盐的I型结晶或权利要求5所述的药物组合物在制备治疗白血病药物中的用途;其中所述的白血病基因靶点为急性髓系AML1-ETO融合基因。
- 根据权利要求1所述的L-丙氨酸-(14-草甲素)酯三氟乙酸盐的I型结晶或权利要求5所述的药物组合物在制备治疗癌症的药物中的用途,其中所述癌症是食道癌、胃癌、原发性肝癌、胰腺癌、贲门癌、大肠癌、膀胱癌、乳腺癌以及急性髓系白血病。
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CN201580002233.8A CN105636964B (zh) | 2014-05-30 | 2015-04-28 | L‑丙氨酸‑(14‑冬凌草甲素)酯三氟乙酸盐的i型结晶及制备方法 |
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CN2014102409200 | 2014-05-30 | ||
CN201410240920.0A CN105131009A (zh) | 2014-05-30 | 2014-05-30 | L-丙氨酸-(14-冬凌草甲素)酯三氟乙酸盐的i型结晶及制备方法 |
PCT/CN2015/077620 WO2015180549A1 (zh) | 2014-05-30 | 2015-04-28 | L-丙氨酸-(14-冬凌草甲素)酯三氟乙酸盐的i型结晶及制备方法 |
CN201580002233.8A CN105636964B (zh) | 2014-05-30 | 2015-04-28 | L‑丙氨酸‑(14‑冬凌草甲素)酯三氟乙酸盐的i型结晶及制备方法 |
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CN105636964B CN105636964B (zh) | 2017-04-12 |
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CN201580002233.8A Active CN105636964B (zh) | 2014-05-30 | 2015-04-28 | L‑丙氨酸‑(14‑冬凌草甲素)酯三氟乙酸盐的i型结晶及制备方法 |
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Citations (4)
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CN101139350A (zh) * | 2007-10-15 | 2008-03-12 | 中国药科大学 | 冬凌草甲素类衍生物、其制备方法及用途 |
CN102058566A (zh) * | 2010-12-24 | 2011-05-18 | 中国药科大学 | 一种冬凌草甲素类成分干粉吸入剂及其制备方法和用途 |
WO2013107429A1 (zh) * | 2012-01-21 | 2013-07-25 | 杭州本生药业有限公司 | 1-氧代/酰化-14-酰化的冬凌草甲素衍生物、及其制备方法和应用 |
CN103467474A (zh) * | 2013-09-17 | 2013-12-25 | 中国药科大学 | 1,6,7,14-位取代的冬凌草甲素衍生物、制备方法及用途 |
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CN104017000B (zh) * | 2013-03-01 | 2017-01-04 | 江苏恒瑞医药股份有限公司 | L-丙氨酸-(14-冬凌草甲素)酯三氟乙酸盐及其制备方法和用途 |
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Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101139350A (zh) * | 2007-10-15 | 2008-03-12 | 中国药科大学 | 冬凌草甲素类衍生物、其制备方法及用途 |
CN102058566A (zh) * | 2010-12-24 | 2011-05-18 | 中国药科大学 | 一种冬凌草甲素类成分干粉吸入剂及其制备方法和用途 |
WO2013107429A1 (zh) * | 2012-01-21 | 2013-07-25 | 杭州本生药业有限公司 | 1-氧代/酰化-14-酰化的冬凌草甲素衍生物、及其制备方法和应用 |
CN103467474A (zh) * | 2013-09-17 | 2013-12-25 | 中国药科大学 | 1,6,7,14-位取代的冬凌草甲素衍生物、制备方法及用途 |
Non-Patent Citations (1)
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冯卫生,等,: "冬凌草化学成分研究进展", 《中国新药杂志》 * |
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CN105636964B (zh) | 2017-04-12 |
CN105131009A (zh) | 2015-12-09 |
HK1223618A1 (zh) | 2017-08-04 |
WO2015180549A1 (zh) | 2015-12-03 |
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Effective date of registration: 20180428 Address after: 222047 No. 7 Kunlun Shan Road, Lianyungang economic and Technological Development Zone, Jiangsu Co-patentee after: Shanghai Sheng Di Medicine Co., Ltd. Patentee after: Hengrui Medicine Co., Ltd., Jiangsu Prov. Address before: 222047 No. 7 Kunlun Shan Road, Lianyungang economic and Technological Development Zone, Jiangsu Patentee before: Hengrui Medicine Co., Ltd., Jiangsu Prov. |