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公开(公告)号：US20190263809A1
公开(公告)日：2019-08-29
申请号：US16405722
申请日：2019-05-07
发明人： Haisheng Fan , Xiaowen Guo , Luning Huang , Hong Gu
IPC分类号： C07D471/04 , B01D9/00
摘要： Disclosed is a preparation method for a Palbociclib free base crystal form A as shown in Formula I, comprising the following steps: treating a Palbociclib free base and/or a Palbociclib salt compound by using an inorganic base in a water solvent at the temperature of 35 to 100′C. to obtain a Palbociclib free base crystal form A, the water solvent being water or mixed solvent obtained by water and an organic solvent capable of being mixed and disclosed in the water. Also disclosed is a preparation method for a Palbociclib free base crystal form B, comprising the following steps: treating a Palbociclib salt compound by using an inorganic base in a water solvent at the temperature of 0 to 20° C. to obtain a Palbociclib free crystal form B, the water solvent being water or a mixed solvent obtained by water and an organic solvent capable of being mixed and dissolved in the water. The method is safe and convenient in operation and low in pollution, and facilitates industrial production.
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公开(公告)号：US10329290B2
公开(公告)日：2019-06-25
申请号：US15772497
申请日：2016-11-02
发明人： Haisheng Fan , Xiaowen Guo , Luning Huang , Hong Gu
IPC分类号： C07D487/04 , C07D471/04 , B01D9/00 , A61K31/519
摘要： Disclosed is a preparation method for a Palbociclib free base crystal form A as shown in Formula I, comprising the following steps: treating a Palbociclib free base and/or a Palbociclib salt compound by using an inorganic base in a water solvent at the temperature of 35 to 100° C. to obtain a Palbociclib free base crystal form A, the water solvent being water or mixed solvent obtained by water and an organic solvent capable of being mixed and disclosed in the water. Also disclosed is a preparation method for a Palbociclib free base crystal form B, comprising the following steps: treating a Palbociclib salt compound by using an inorganic base in a water solvent at the temperature of 0 to 20° C. to obtain a Palbociclib free crystal form B, the water solvent being water or a mixed solvent obtained by water and an organic solvent capable of being mixed and dissolved in the water. The method is safe and convenient in operation and low in pollution, and facilitates industrial production.
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公开(公告)号：US12116342B2
公开(公告)日：2024-10-15
申请号：US17312195
申请日：2019-12-12
发明人： Haisheng Fan , Yipeng Zhan , Kai Yin , Xiang Ji , Fenghao Liu , Kaiqiang Shi , Xiaowen Guo , Luning Huang , Anping Tao , Jianguo An , Hong Gu
IPC分类号： C07D207/27
CPC分类号： C07D207/27 , C07B2200/07 , C07B2200/13
摘要： The present application relates to a method (I) for preparing a brivaracetam intermediate, comprising the steps of dissolving the compound represented by B-P and 1S,2S-diphenylethylenediamine in a solvent for resolution, crystallizing, filtering, and recrystallizing to obtain the compound represented by B-Q, which is then converted to the brivaracetam intermediate represented by B-R. This method can effectively resolve the compound represented by B-P. The present application also provides a method for preparing brivaracetam using the compound represented by B-R. The method can separate the effective components only through simple steps such as extraction, washing, drying, and concentration without requiring use of chiral chromatography column to separate isomers in the preparation process, and thus the separation process is simple, greatly reducing the production cost of brivaracetam.
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公开(公告)号：US10766895B2
公开(公告)日：2020-09-08
申请号：US16405722
申请日：2019-05-07
发明人： Haisheng Fan , Xiaowen Guo , Luning Huang , Hong Gu
IPC分类号： C07D487/04 , C07D471/04 , B01D9/00 , A61K31/519
摘要： Disclosed is a preparation method for a Palbociclib free base crystal form A as shown in Formula I, comprising the following steps: treating a Palbociclib free base and/or a Palbociclib salt compound by using an inorganic base in a water solvent at the temperature of 35 to 100′C. to obtain a Palbociclib free base crystal form A, the water solvent being water or mixed solvent obtained by water and an organic solvent capable of being mixed and disclosed in the water. Also disclosed is a preparation method for a Palbociclib free base crystal form B, comprising the following steps: treating a Palbociclib salt compound by using an inorganic base in a water solvent at the temperature of 0 to 20° C. to obtain a Palbociclib free crystal form B, the water solvent being water or a mixed solvent obtained by water and an organic solvent capable of being mixed and dissolved in the water. The method is safe and convenient in operation and low in pollution, and facilitates industrial production.
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公开(公告)号：US20180319790A1
公开(公告)日：2018-11-08
申请号：US15772497
申请日：2016-11-02
发明人： Haisheng Fan , Xiaowen Guo , Luning Huang , Hong Gu
IPC分类号： C07D471/04 , B01D9/00
CPC分类号： C07D471/04 , A61K31/519 , B01D9/0054 , B01D9/0063
摘要： Disclosed is a preparation method for a Palbociclib free base crystal form A as shown in Formula I, comprising the following steps: treating a Palbociclib free base and/or a Palbociclib salt compound by using an inorganic base in a water solvent at the temperature of 35 to 100° C. to obtain a Palbociclib free base crystal form A, the water solvent being water or mixed solvent obtained by water and an organic solvent capable of being mixed and disclosed in the water. Also disclosed is a preparation method for a Palbociclib free base crystal form B, comprising the following steps: treating a Palbociclib salt compound by using an inorganic base in a water solvent at the temperature of 0 to 20° C. to obtain a Palbociclib free crystal form B, the water solvent being water or a mixed solvent obtained by water and an organic solvent capable of being mixed and dissolved in the water. The method is safe and convenient in operation and low in pollution, and facilitates industrial production.
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