High-purity ranolazine and preparation method thereof

A ranolazine and high-purity technology, applied in the field of high-purity ranolazine and its preparation, can solve the problems of complicated operation, high operation cost, long steps and the like, and achieve the effects of good appearance and high purity

Inactive Publication Date: 2009-10-21
BEIJING WANQUAN SUNSHINE MEDICAL TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] EP0126449 reports two synthetic routes of ranolazine, but the operation is cumbersome and unfavorable for industrialized production
The refining of ranolazine has no relevant reports, and some documents disclose the method of refining after obtaining ranolazine hydrochloride, but the operation cost is high, the yield is low, and the steps are long

Method used

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  • High-purity ranolazine and preparation method thereof
  • High-purity ranolazine and preparation method thereof
  • High-purity ranolazine and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] In a 20L three-neck flask, add 7L of ethanol and 1.4kg (11.5mol) of 2,6-dimethylaniline respectively, and add 1.4kg (13.8mol) of triethylamine at temperature control T=10°C-20°C. Temperature control T=10°C-20°C, 1.9 kg (17.3 mol) of chloroacetyl chloride was added dropwise. After dropping, the temperature was controlled at T=10°C to 20°C to continue the reaction for 2 hours. Add distilled water, stir, and filter with suction. The filter cake was air-dried at 60° C. for 12 hours to obtain 2.0 kg of N-(2,6-dimethylphenyl)chloroacetamide off-white solid, yield: 90%.

Embodiment 2

[0034] In a 20L three-neck flask, add 7L of isopropanol and 1.4kg (11.5mol) of 2,6-dimethylaniline respectively, and add 1.4kg (13.8mol) of triethylamine at temperature control T=10°C-20°C. Temperature control T=10°C-20°C, 1.9 kg (17.3 mol) of chloroacetyl chloride was added dropwise. After dropping, the reaction was continued for 2 hours under temperature control T=0°C-10°C. Add distilled water, stir, and filter with suction. The filter cake was air-dried at 60° C. for 12 hours to obtain 2.06 kg of N-(2,6-dimethylphenyl)chloroacetamide off-white solid, yield: 94%.

Embodiment 3

[0036] Into a 20L three-necked flask, add 12L of toluene and 2.4kg (12.1mol) of N-(2,6-dimethylphenyl)chloroacetamide, respectively. Add 9.4 kg (48.5 mol) of piperazine hexahydrate under stirring, and heat to reflux for 4 hours. Stop the reaction, spin out the solvent under reduced pressure, and add ethyl acetate to dissolve. Suction filtration, the filtrate spins off the solvent under reduced pressure. Add isopropyl ether and beat for 0.5 hours. After suction filtration, the filter cake was air-dried at 60° C. for 8 hours to obtain 2.5 kg of N-(2,6-dimethylphenyl)-1-piperazineacetamide as a white solid, yield: 84%.

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Abstract

The invention discloses a preparation technology and a refining method of ranolazine, which are more suitable for industrial production. The method comprises the following concrete steps: using 2, 6-dimethylaniline and methylpyrocatechine as original materials; sequentially carrying out four reaction processes of N-acylation, O-alkylation, N-alkylation and N-alkylation to synthesize ranolazine; and then, recrystallizing to obtain a refined product. The refined product obtained by the method has high purity, and the method also has the advantages of simple operation, low production cost and high yield and is more suitable for industrial production.

Description

technical field [0001] The invention relates to a high-purity ranolazine and a preparation method thereof. Background technique [0002] Ranolazine (±)-N-(2,6-dimethylphenyl)-4-[2-hydroxy-3-(2-methoxyphenoxy)propyl]-1-piper Azineacetamide ((±)-N-(2,6-Dimethylphenyl)-4-[2-hydroxy-3-(2-methoxyphenoxy)propyl]-1-piperazineacetamide) has the following structure: [0003] [0004] Ranolazine is a new type of drug for the treatment of angina-type coronary heart disease developed by CV Therapeutics of the United States. It is called a pFOX (partial fatty acid oxidation) inhibitor and is the only anti-angina drug that does not cause changes in heart rate and blood pressure. [0005] EP0126449 reports two synthetic routes of ranolazine, but the operation is cumbersome and unfavorable for industrial production. There is no relevant report on the purification of ranolazine, and there are literatures disclosing a method for refining after obtaining ranolazine hydrochloride, but the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D295/15A61P9/10
Inventor 王世峰谌伦华刘国旗焦育红陈年根
Owner BEIJING WANQUAN SUNSHINE MEDICAL TECH CO LTD
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