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A crystal form of palbociclib dihydrochloride and a preparing method thereof

A technology of dihydrochloride and crystal form, which is applied in the field of compositions containing the solid form, can solve the problems of low bioavailability, poor water solubility, etc., and achieve the effects of simple preparation method, not easy to absorb moisture, and stable crystal form

Inactive Publication Date: 2017-06-06
SHANGHAI SYNCORES TECH INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The labeling also states that palbociclib free base has poor water solubility and has low bioavailability in animal studies, while palbociclib dihydrochloride appears to be sufficiently water soluble but not hygroscopic. Studies have shown that even at low relative humidity (10% RH), the dihydrochloride still absorbs more than 2% of its mass of water, making it unsuitable for use in solid pharmaceutical products

Method used

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  • A crystal form of palbociclib dihydrochloride and a preparing method thereof
  • A crystal form of palbociclib dihydrochloride and a preparing method thereof
  • A crystal form of palbociclib dihydrochloride and a preparing method thereof

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Embodiment 1

[0028] Example 1: 6-acetyl-8-cyclopentyl-5-methyl-2-[[5-(piperazin-1-yl)pyridin-2-yl]amino]-8H-pyrido[2, Preparation of 3-D]pyrimidin-7-one dihydrochloride

[0029] Take 100g 4-[6-[(6-(1-butoxyethenyl)-8-cyclopentyl-7,8-dihydro-5-methyl-7-oxopyrido[2,3-D ]pyrimidin-2-yl)amino]-3-pyridyl]-1-piperazinecarboxylate tert-butyl into a 2L three-neck flask, add 1.0L methanol, 41.5ml hydrochloric acid, 100ml water. Heat to about 60-65°C and stir for 3-4 hours. The system was cooled to 0-5°C, crystallized, and a yellow solid was obtained by suction filtration. The resulting solid was recrystallized and purified in a mixed solvent of methanol and water, and dried to obtain 63.4 g (72.4% yield) of light yellow fluffy solid, with an HPLC purity of 99.8%.

[0030] Physical parameters: Ms, melting point and infrared, etc.

[0031] Using 6-acetyl-8-cyclopentyl-5-methyl-2-[[5-(piperazin-1-yl)pyridin-2-yl]amino]-8H-pyrido[2 ,3-D]pyrimidin-7-one dihydrochloride (compound of formula Ⅰ) new c...

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Abstract

The invention discloses a novel crystal form of 6-acetyl-8-cyclopentyl-5-methyl-2-[[5-(piperazin-1-yl)pyridin-2-yl]amino]-8H-pyrido[2,3-D]pyrimidin-7-one dihydrochloride, a medicine composition thereof and a preparing method of the crystal form. The dihydrochloride crystal form is good in stability. The preparing method is simple and easy to operate.

Description

technical field [0001] The present invention relates to a compound containing 6-acetyl-8-cyclopentyl-5-methyl-2-[[5-(piperazin-1-yl)pyridin-2-yl]amino]-8H-pyrido[2, 3-d] Solid forms of pyrimidin-7-one dihydrochloride, and compositions comprising such solid forms; [0002] technical background [0003] 6-Acetyl-8-cyclopentyl-5-methyl-2-[[5-(piperazin-1-yl)pyridin-2-yl]amino]-8H-pyrido[2,3-d] Pyrimidin-7-one, a selective, once-daily cyclin-dependent kinase (CDK) 4 / 6 inhibitor developed by Pfizer, in postmenopausal women with ER-positive, HER2-negative forms of advanced breast cancer It has shown strong efficacy and has been certified by the FDA as a breakthrough drug. On February 3, 2015, the drug was approved for marketing in the United States. [0004] WO2003062236 Example 36 discloses 6-acetyl-8-cyclopentyl-5-methyl-2-[[5-(piperazin-1-yl)pyridin-2-yl]amino]-8H-pyrido[ 2,3-d] The preparation method of pyrimidin-7-one hydrochloride, by passing hydrogen chloride gas into 4-...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D471/04A61K31/519A61P35/00
CPCC07B2200/13C07D471/04
Inventor 樊海生郭效文黄鲁宁顾虹
Owner SHANGHAI SYNCORES TECH INC