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Preparation method of palbociclib free base with small specific surface area

A specific surface area and free alkali technology, applied in organic chemistry and other fields, can solve problems such as poor fluidity, small product particle size, and poor stability

Active Publication Date: 2018-05-11
SHANGHAI ACEBRIGHT PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Since this crystal form is a solvate, the solvent content is high, the stability is poor, and the product has a small particle size and poor fluidity, so it cannot be used as a raw material drug to make a preparation

Method used

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  • Preparation method of palbociclib free base with small specific surface area
  • Preparation method of palbociclib free base with small specific surface area
  • Preparation method of palbociclib free base with small specific surface area

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preparation example Construction

[0066] Preparation of Palbociclib Free Base with Small Specific Surface Area

[0067] The invention provides a method for preparing palbociclib free base with a small specific surface area, the method comprising the following steps (a)-(c):

[0068] (a) dissolving palbociclib and / or its salt in a solvent to obtain a solution system containing palbociclib or its salt; wherein, the solvent includes an organic solvent, and optional water;

[0069] In the step (a), the dissolution may use an organic solvent, or a mixed solvent of an organic solvent and water. In a preferred embodiment, the volume ratio of the organic solvent to water is 15-1.25:1, preferably 14-3:1, more preferably 13-5:1. The organic solvent can be a commonly used solvent for preparing pharmaceutically acceptable crystals, for example, a solvent selected from the group consisting of C1-C6 alcohols, C3-C7 ketones, N,N-dimethylformaldehyde Amide, N,N-dimethylacetamide, tetrahydrofuran, or a combination thereof. ...

Embodiment 11

[0119] Mix 10g of palbociclib dihydrochloride with 200mL of methanol and 20mL of water into a three-necked flask, heat and stir to dissolve, heat up the filtrate to 63°C, and the pH is about 1.5-3, start Slowly add 0.25mol / Na 2 CO 3 Adjust the pH of the solution to >9, and keep stirring at 63° C. for 1 h. Slowly lower the temperature to 0-5° C., and stir at this temperature for 1 h; finally, the precipitated crystals are collected by filtration, washed with water, and dried to obtain 8.7 g of crystals with a molar yield of 94%.

Embodiment 12

[0121] Mix 10g of palbociclib monohydrochloride with 180mL of methanol and 20mL of water in a three-necked flask, heat and stir to dissolve, heat up the filtrate to 55°C, and the pH is about 1.5-3, start Slowly add 0.25mol / Na 2 CO 3 Adjust the pH of the dissolved solution to >9, heat up to 60°C and keep stirring for 1h. Slowly lower the temperature to 0-5° C., and stir at this temperature for 1 h; finally, the precipitated crystals are collected by filtration, washed with water, and dried to obtain 8.5 g of crystals with a molar yield of 94%.

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Abstract

The invention provides a simple, safe and easily operable preparation method of palbociclib free base with small specific surface area. Specifically, the preparation method of the invention includes the steps of: dissolving palbociclib and / or its salt in a mixed solvent of an organic solvent and water to form a solution system, heating the solution system to 30-70DEG C, adding lye into the solution system, cooling the solution system, and performing filtering to obtain the palbociclib free base with small specific surface area.

Description

technical field [0001] The invention belongs to the technical field of medicinal chemistry, and in particular relates to a preparation method of palbociclib free base with small specific surface area. Background technique [0002] Compound 6-acetyl-8cyclopentyl-5-methyl-2-(5-piperazin-1-yl-pyridin-2-ylamino)-8H-pyrido[2,3-d]pyrimidine-7 - Ketone (palbociclib free base), the chemical structural formula is: [0003] [0004] The compound is a breast cancer drug developed by Pfizer. It was approved for marketing in the United States in April 2015. The dosage form of the drug is capsules. [0005] According to the description in International Patent Application Publication WO 2005 / 005426, the free base provided by the traditional salt fragmentation procedure is very prone to static electricity and forms small primary particles that coalesce into large, hard agglomerates, which Agglomerates are difficult to disperse by sieving and have strong stickiness after impact, which i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D471/04
CPCC07D471/04
Inventor 安晓霞申淑匣詹小兰谢相雨
Owner SHANGHAI ACEBRIGHT PHARMA CO LTD
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