Method for preparing lidocaine through continuous reaction

A technology for lidocaine and dimethylaniline, which is applied in the field of continuous reaction preparation of lidocaine, can solve the problems of excessive residue, high cost of raw materials, complicated process operation, etc., and achieves reduction of sewage discharge, reduction of production cost, and simplification of process effect of operation

Active Publication Date: 2020-12-15
山东诚汇双达药业有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This technical solution mainly has the following defects: (1) In this method, acetone is used as a solvent to prepare lidocaine, and in the next step reaction, diethylamine is reacted, and the solvent cannot be recovered and applied mechanically
(2) Petroleum ether is used for secondary recrystallization in this method, resulting in higher cost of raw materials
(3) In this method, a one-pot method is used to prepare lidocaine, and the yield is only 82%, which is relatively low
(4) There is no process of washing with water to completely remove inorganic salts during the reaction, which will cause the residue to exceed the standard
In this method, there are following defects: (1) the raw materials N,N-diethylaminoacetate methyl ester and 5%Pd/C used as the main catalyst are expensive,

Method used

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  • Method for preparing lidocaine through continuous reaction

Examples

Experimental program
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Effect test

Example Embodiment

[0032]Example 1

[0033]Put 300kg of 2,6-dimethylaniline and 1500kg of ethyl acetate into the reactor and stir; add 307kg of chloroacetyl chloride dropwise, and after the dropwise addition is completed, the temperature is raised to 70-75℃, and the generated hydrogen chloride gas is absorbed by deionized water as Dilute hydrochloric acid, apply it to the next step to adjust the acid; stir the reaction for 1 hour until the reaction is complete, reduce the temperature to 50 ℃, add 520 kg of sodium carbonate, 15 kg of potassium iodide, 2400 kg of water, add 430 kg of diethylamine, add 430 kg, and increase the temperature to 70 ℃ until the reaction When finished, cool down to normal temperature; stand still, separate the liquids, adjust the pH to 3.0-4.0 with the dilute hydrochloric acid absorbed by the tail gas before adding the ethyl acetate layer, extract, stand still, and separate; the organic layer recovers ethyl acetate; the water layer is added with activated carbon to decolorize and...

Example Embodiment

[0034]Example 2

[0035]Put 100kg of 2,6-dimethylaniline and 500kg of toluene into the reactor and stir; add 102.5kg of chloroacetyl chloride dropwise, and the addition will be completed in about 2 hours; increase the internal temperature to 80-90℃, use deionized water Absorb the generated hydrogen chloride gas as dilute hydrochloric acid and apply it to the next step to adjust the acid; stir the reaction for 1 hour until the reaction is complete, add 175kg of sodium carbonate, 5kg of potassium iodide, and 800kg of water, continue to stir for 0.5 hours until the mixture is uniform; add 145kg of diethylamine, It takes about 0.5-1 hours to complete the addition; keep the reaction for 6-9 hours until the reaction is complete, and cool to room temperature; stand still for 0.5-1 hour; separate liquids, adjust the pH to 2.0-4.5 by adding dilute hydrochloric acid absorbed by the tail gas before the toluene layer is added, and stir and extract. Let stand for 30 minutes and separate; the organi...

Example Embodiment

[0036]Example 3

[0037]Put 300kg of 2,6-dimethylaniline and 1500kg of ethyl acetate into the reactor and stir; start dripping 307kg of chloroacetyl chloride, and the dripping is complete; increase to the internal temperature of 70-75℃, and absorb the resulting product with deionized water Hydrogen chloride gas is used as dilute hydrochloric acid, applied to the next step to adjust the acid; stir the reaction for 1 hour until the reaction is complete, cool to 40-60 ℃, add 515kg potassium carbonate, 9kg potassium iodide, 2400kg water, add 362kg diethylamine, and increase the temperature to 65 -75°C until the reaction is complete, cool to room temperature; stand still, separate the liquids, adjust the pH to 3.0-3.5 by adding the dilute hydrochloric acid absorbed by the tail gas before the ethyl acetate layer, extract, stand still, and separate; the organic layer recovers ethyl acetate; the water layer Add activated carbon to decolorize and filter. The filtrate is adjusted to pH=8.5-9.0 w...

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Abstract

The invention belongs to the technical field of chemical synthesis, and particularly relates to a method for preparing lidocaine through continuous reaction. According to the method, a continuous reaction method is adopted, crystallization, separation, purification and other treatment and drying processes of an intermediate chloroacetyl -2, 6-dimethylaniline are not needed, a lidocaine finished product can be directly obtained, and the molar yield is 93% or above. The process operation is simplified, the solvent is recycled, the sewage discharge amount is reduced, the production cost is reduced, energy conservation and consumption reduction are realized, and the process is green and environment-friendly.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a method for preparing lidocaine through continuous reaction. Background technique [0002] Lidocaine, chemical name: N-(2,6-xylyl)-2-(diethylamino)acetamide, English name: Lidocaine. Lidocaine is a local anesthetic commonly used in medical clinics. 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 diseases complicated by rapid ventricular arrhythmia. Drug of choice for tachycardia and ventricular tremor. [0003] The synthetic method of lidocaine in the prior art mainly contains at present: [0004] Patent CN102070483A discloses a method for preparing lidocaine, which involves a one-pot method for preparing lidocaine. The specific content is: add 305g of 2,6-dimethylaniline to a 5000mL three-necked bottle, and use 2000mL of acetone to prepare Solvent, then ad...

Claims

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Application Information

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IPC IPC(8): C07C237/04C07C231/12C07C231/24
CPCC07C231/12C07C231/02C07C231/24C07C237/04C07C233/07
Inventor 王延斌张健隋海超李跃东黄凤芸任真真
Owner 山东诚汇双达药业有限公司
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