Preparation method of lidocaine hydrochloride impurity E

A technology for lidocaine hydrochloride and impurities, which is applied in the field of compound synthesis technology, can solve the problem of not synthesizing lidocaine hydrochloride impurity E and the like, and achieves the effects of high purity, safe reaction and high yield

Active Publication Date: 2020-11-27
ZHENGZHOU SIGMA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] There is no method for synthesizing lidocaine hydrochloride impurity E in the prior art

Method used

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  • Preparation method of lidocaine hydrochloride impurity E
  • Preparation method of lidocaine hydrochloride impurity E
  • Preparation method of lidocaine hydrochloride impurity E

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] The preparation method of the lidocaine hydrochloride impurity E of the present embodiment comprises the following steps: add 20g of compound 1, i.e. 4-morpholine-3-aniline, and 35ml of solvent DMF to a reactor with a thermometer and a stirring paddle , and then add 21.1 g of compound 2a, namely 2-chloro-N-(2,6-xylyl) acetamide, under stirring conditions at room temperature, and after stirring for 30 min, add 12.3 g of diethylamine, and react for 40 min at 25°C , raised the temperature to 60°C for 2 hours, then raised the temperature to 90°C for 3 hours, added water and ethyl acetate, washed the organic layer with saturated brine, dried over anhydrous sodium sulfate, filtered, and removed the solvent in vacuo to obtain 31.2 g of lidocaine hydrochloride Impurity E has a purity of 98.2% and a yield of 89.2%. The reaction formula is shown in formula 2.

[0026]

Embodiment 2

[0028] The preparation method of the lidocaine hydrochloride impurity E of the present embodiment comprises the steps of: adding 20 g of compound 1, i.e. 4-morpholine-3-aniline, and 35 ml of solvent two to a reactor with a thermometer and a stirring paddle Chloromethane, then add 32.6g of compound 2b, namely 2-bromo-N-(2,6-xylyl)acetamide, under stirring at room temperature, and after stirring for 20min, add 28.9g of N,N-diisopropyl Ethylamine, react at 30°C for 50min, raise the temperature to 45°C for 3h, then raise the temperature to 100°C for 2h, add water and ethyl acetate, wash the organic layer with saturated saline, dry over anhydrous sodium sulfate, filter, and remove the solvent in vacuo , to obtain 34.1 g of lidocaine hydrochloride impurity E, with a purity of 98.6% and a yield of 88.2%. The reaction formula is shown in formula 3.

[0029]

Embodiment 3

[0031] The preparation method of the lidocaine hydrochloride impurity E of the present embodiment comprises the following steps: add 20g of compound 1, i.e. 4-morpholine-3-aniline, and 35ml of solvent DMSO to a reactor with a thermometer and a stirring paddle , and then added 32.4 g of compound 2c, namely 2-methoxy-N-(2,6-xylyl) acetamide, under stirring conditions at room temperature, and after stirring for 40 min, added 34.0 g of triethylamine, at 30 ° C React for 30 minutes, raise the temperature to 45°C for 1.5h, then raise the temperature to 80°C for 4h, add water and ethyl acetate, wash the organic layer with saturated brine, dry over anhydrous sodium sulfate, filter, and remove the solvent in vacuo to obtain 35.0g of hydrochloric acid Lidocaine impurity E has a purity of 98.0% and a yield of 90.6%. The reaction formula is shown in formula 4.

[0032]

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Abstract

The invention relates to a preparation method of a lidocaine hydrochloride impurity E, and belongs to the technical field of compound synthesis processes. The preparation method of the lidocaine hydrochloride impurity E comprises the following steps that: 4-morpholine-3-aniline is dissolved in a solvent; then an obtained solution reacts with substituted 2, 6-dimethylphenyl acetamide under the action of an acid-binding agent to generate the lidocaine hydrochloride impurity E. The lidocaine hydrochloride impurity E with higher purity can be obtained, the yield of the lidocaine hydrochloride impurity E is higher, and the purification steps are fewer.

Description

technical field [0001] The invention belongs to the technical field of compound synthesis technology, and in particular relates to a preparation method of lidocaine hydrochloride impurity E. Background technique [0002] Lidocaine is an anesthetic and antiarrhythmic drug that has been clinically used for many years. It was synthesized by Lofgren in 1934 and is used as a local anesthetic. It is a derivative of cocaine, but it does not have hallucinations and addiction. Components, local anesthesia has a strong and long-lasting effect, and has good surface penetration. It can be injected or used as a topical anesthesia. It usually takes effect within one to three minutes after application, and the effect lasts for one to three hours. In the 1950s, it was used to treat ventricular arrhythmia that occurred during the operation. It was used to treat arrhythmia in 1963. It is currently a drug for the prevention and treatment of acute myocardial infarction and various heart disease...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C231/12C07C237/04
CPCC07C231/12C07C237/04
Inventor 汪游清张高锋张颖申丽坤肖楚晖
Owner ZHENGZHOU SIGMA CHEM
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