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A kind of preparation method of plerixafor impurity

A technology of plerixafor and impurities, which is applied in the direction of organic chemistry, can solve the problems of unreported compound research, and achieve the effects of simple and easy reagents, strong operability, and reasonable synthesis process design

Active Publication Date: 2019-12-06
TLC NANJING PHARMA RANDD CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] This compound is a common impurity in the synthesis process of plerixafor, which can provide a control sample for the quality control of the raw material plerixafor, but the research on this compound has not been reported at home and abroad

Method used

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  • A kind of preparation method of plerixafor impurity
  • A kind of preparation method of plerixafor impurity
  • A kind of preparation method of plerixafor impurity

Examples

Experimental program
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Effect test

Embodiment 1

[0031] (1) Dissolve 10.00 g of 1,4,8,11-tetraazacyclotetradecane in 1 L of dry dichloromethane, add 15.3 mL of pyridine and 14.28 g of p-toluenesulfonyl chloride under ice-cooling to obtain a colorless solution , react overnight at 30°C. The reaction solution was directly spin-dried and then purified by chromatographic column to obtain 20.5 g of compound IV as a white foamy solid, with a yield of 80.74%;

[0032] (2) Dissolve 30.00g of 1,4,8,11-tetraazacyclotetradecane in 150mL of methanol, add 21.6mL of triethylamine, add 53.19g of trifluoroacetic acid dropwise with a constant pressure dropping funnel under ice bath Ethyl ester, the solution was clear, reacted overnight at 30°C, the reaction solution was spin-dried and purified by chromatographic column to obtain 60 g of compound III as a colorless oily liquid, with a yield of 82.04%;

[0033] (3) Dissolve 30 g of the compound III in 150 mL of acetonitrile, and add 64.86 g of compound V and 8.73 g of K 2 CO 3 , was a white...

Embodiment 2

[0039] (1) Dissolve 30.0 g of 1,4,8,11-tetraazacyclotetradecane in 1 L of dry dichloromethane, add 52 mL of triethylamine and 48.5 g of p-toluenesulfonyl chloride under ice-cooling to obtain a colorless solution, reacted at 30°C for 10 hours. The reaction solution was directly spin-dried and then purified by chromatographic column to obtain 62 g of compound IV as a white foamy solid, with a yield of 81.39%;

[0040] (2) Dissolve 40.0g of 1,4,8,11-tetraazacyclotetradecane in 200mL of methanol, add 40mL of triethylamine, add 79.4g of ethyl trifluoroacetate dropwise with a constant pressure dropping funnel under ice-cooling Ester, the solution was clear, reacted at 30°C for 8 hours, the reaction solution was spin-dried and purified by chromatographic column to obtain 85 g of compound III colorless oily liquid, with a yield of 87.17%;

[0041] (3) Dissolve 20g of the compound III in 100mL of acetonitrile, and add 21.62g of compound V and 5.8g of K 2 CO 3 , was a white suspensio...

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Abstract

The invention discloses a preparation method of a plerixafor impurity and belongs to the field of medicine synthesis. By adopting the preparation method, a product with the purity reaching 99.16 percent can be obtained; a technology is simple in design and strong in operability and industrial production can be realized. The preparation method takes 1,4,8,11-tetraazacyclotetradecane as a raw material and realizes the synthesis of the plerixafor impurity through seven-step reaction; the plerixafor impurity prepared by the preparation method disclosed by the invention provides important evidencesfor carrying out scientific evaluation on quality, safety and efficiency of the plerixafor.

Description

technical field [0001] The invention belongs to the field of drug synthesis, in particular to a method for preparing plerixafor impurities. Background technique [0002] Plerixafor is a drug that can increase the number of hematopoietic stem cells. It is mainly used for adult tumor patients such as multiple myeloma and non-Hodgkin's lymphoma who have received stem cell bone marrow transplantation. It is in the form of white solid powder and is used for medicinal purposes. In the form of injection, the chemical name is 1,1'-[1,4-phenylenebis(methylene)]-bis-1,4,8,11-tetraazacyclotetradecane, and the molecular weight is: 502.80, the structural formula is: [0003] [0004] With the advancement of the times and the improvement of the level of science and technology, people have a fuller understanding of the quality, safety and efficacy of drugs. Among them, drug impurities are directly related to the quality and safety of drugs. and types are strictly regulated. An impuri...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D257/02
Inventor 杨石张海林张池王忠义崔希林
Owner TLC NANJING PHARMA RANDD CO LTD
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