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Preparation method of Palbociclib isethionate

A technology of isethionate and ethyl acetate, applied in the field of chemical drug synthesis, can solve the problems of unsuitability for industrial production, high production cost, long synthesis steps, etc., and achieves avoiding metal catalysts, reducing reaction costs and process conditions. mild effect

Inactive Publication Date: 2016-05-04
NANJING CORE TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0018] The method uses compound 1, compound 2 and compound 4 as raw materials to synthesize fragment compound B and compound C. The method uses a Pd / C (palladium carbon) metal catalyst in the preparation process, and the synthesis steps are long and the total yield is low. Production High cost, not suitable for industrial production

Method used

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  • Preparation method of Palbociclib isethionate
  • Preparation method of Palbociclib isethionate
  • Preparation method of Palbociclib isethionate

Examples

Experimental program
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Embodiment 1

[0040] A preparation method of isethionate palbociclib (Palbociclib), comprising the following steps:

[0041] (1) Substituting the compound shown in formula B with the compound shown in formula C to obtain the compound shown in formula D:

[0042]

[0043]Put 810g (2.91mol) of compound B and 3.0LTHF into a 10L three-necked flask, evacuate and replace with nitrogen three times, stir at 20°C for 30 minutes, then slowly add 1.2L isopropylmagnesium chloride (2.0MinTHF) dropwise to the system, and keep warm at 20°C Stir for 1 hour, put 770g (2.25mol) of compound C into the system, evacuate nitrogen for 3 times, slowly add 1.2L isopropylmagnesium chloride (2.0MinTHF) dropwise to the system, after the dropwise addition, raise the temperature to 60°C The reaction was stirred, and the progress of the reaction was monitored by TLC. After the reaction, add 1.3L acetic acid and 1.3LTHF (tetrahydrofuran) mixed solution to the reaction solution, solids are precipitated, filtered by suc...

Embodiment 2

[0060] (1) Substituting the compound shown in formula B with the compound shown in formula C to obtain the compound shown in formula D:

[0061]

[0062] Put 810g (2.91mol) of compound B and 3.9LTHF into a 10L three-necked bottle, vacuum nitrogen replacement 3 times, stir at 20°C for 30 minutes, then slowly add 1.2L isopropylmagnesium chloride (2.0MinTHF) dropwise to the system, and keep warm at 20°C Stir for 1 hour, put 770g (2.25mol) of compound C into the system, evacuate nitrogen for 3 times, slowly add 1.2L isopropylmagnesium chloride (2.0MinTHF) dropwise to the system, after the dropwise addition, raise the temperature to 70°C The reaction was stirred, and the progress of the reaction was monitored by TLC. After the reaction, add 1.3L acetic acid and 1.3LTHF (tetrahydrofuran) mixed solution to the reaction solution, solids are precipitated, filtered by suction, the filter cake is beaten once with acetone, water, and acetone respectively, and air-dried at 50 ° C. The c...

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Abstract

The invention belongs to the field of chemical medicine synthesis technology, and more specifically relates to a preparation method of Palbociclib isethionate. The method comprises four steps and is used for preparing Palbociclib, that is 2-(pyridin-2-ylamino)-pyrido[2,3-d]pyrimidin-7-one isethionate. The method has the advantages of mild process conditions, simple post-treatment, high purity, low reaction cost, and easy industrial production.

Description

technical field [0001] The invention belongs to the technical field of chemical drug synthesis, and in particular relates to a preparation method of isethionate palbociclib. Background technique [0002] Palbociclib (Palbociclib) is a new oral targeted agent developed by Pfizer, which can selectively inhibit cyclin-dependent kinase 4 and 6 (CDK4 / 6), restore cell cycle control, and block tumor cell proliferation , FDA (US Food and Drug Administration) granted Breakthrough Therapy Designation for Palbociclib in the treatment of advanced or metastatic ER+ / HER2- breast cancer in April 2013. [0003] The female mammary gland is composed of skin, fibrous tissue, mammary glands and fat. Breast cancer is a malignant tumor that occurs in the mammary gland epithelial tissue. 99% of breast cancers occur in women and only 1% in men. Early breast cancer often does not have typical symptoms and signs, and it is not easy to attract attention. It is often found through physical examinatio...

Claims

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Application Information

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IPC IPC(8): C07D471/04
CPCC07D471/04
Inventor 王雪根何凌云余洋金皓杰郭莉芹
Owner NANJING CORE TECH CO LTD
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