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Green industrial production method of baclofen

A baclofen and green technology, applied in the field of producing GABA derivatives, can solve the problems of unsuitability for industrialized production, toxicity of raw materials and reagents, high cost of raw materials, etc., and achieve short production cycle, high reaction yield and high total yield Effect

Inactive Publication Date: 2016-12-07
ANHUI YIXINMING PHARMA TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0019] This method also requires high-pressure hydrogenation, and at the same time, the pollution is serious, so it is not suitable for industrial production
[0020] At present, all disclosed baclofen production processes have high cost of raw materials, cumbersome routes, complicated operations, high toxicity of raw materials and reagents, and serious environmental pollution, which is not the best choice for industrial production

Method used

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  • Green industrial production method of baclofen

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] a. Preparation of Intermediate II:

[0049] 105g (0.75mol) of p-chlorobenzaldehyde, 400ml of deionized water, 137g (1.05mol) of ethyl acetoacetate, stirred at 15-20°C, slowly drop into 132ml of an aqueous solution of 13.2g (0.1mol) of diammonium hydrogen phosphate , the dropping was completed, kept stirring for 5 hours, filtered, washed the solid with appropriate amount of water, and dried under vacuum at 45-55°C for 4 hours to obtain white solid intermediate II, which was directly used in the next step.

[0050] b. Preparation of Intermediate III:

[0051] Intermediate Ⅱ, potassium hydroxide aqueous solution 420ml (30N), stirred and hydrolyzed at 85-90°C for 2h, TLC identification of the reaction end point (developing solvent: ethyl acetate-petroleum ether=2:3), after the reaction was completed, cooled to At room temperature, add 400ml of dichloromethane and 500ml of deionized water, stir for 20min, let stand to separate layers, discard the organic layer and recover i...

Embodiment 2

[0064] a. Preparation of Intermediate II:

[0065] 105g (0.75mol) of p-chlorobenzaldehyde, 137g (1.05mol) of ethyl acetoacetate, 63g (0.5mol) of melamine, ground at room temperature for 1 hour, after the reaction was completed, 700ml of ethyl acetate was added, stirred for 20 minutes, filtered, the filtrate was concentrated to dryness, solid Wash with an appropriate amount of water, and dry under vacuum at 45-55°C for 4 hours to obtain intermediate II as a white solid, which is directly used in the next step.

[0066] b. Preparation of Intermediate III:

[0067] Intermediate Ⅱ, potassium hydroxide aqueous solution 370ml (30N), stirred and hydrolyzed at 85-90°C for 2h, TLC identification of the reaction end point (developing agent: ethyl acetate-petroleum ether=2:3), after the reaction was completed, cooled to At room temperature, add 400ml of dichloromethane and 400ml of deionized water, stir for 20min, let stand to separate layers, discard the organic layer and recover it, u...

Embodiment 3

[0075] Ethyl cyanoacetate was used to replace step a of Example 1 to prepare intermediate II, and the rest of the steps were the same to obtain 32 g of baclofen with a yield of 78.5%, mp: 205.8-206.3°C, and HPLC content of 99.9%.

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Abstract

The invention discloses a green industrial production method of baclofen and belongs to the technical field of medicine synthesis. The method is carried out with p-chlorobenzaldehyde as an initial raw material and includes five reactions of Knoevenagel condensation, alkaline hydrolysis, imidation, alkaline hydrolysis, and Hofmann degradation, thus preparing the baclofen satisfying clinical medicinal application. The method employs raw materials being very easy to obtain and being low in cost and is simple in synthesis operations, wherein the reactions are carried out under aqueous conditions. The method is very low in environment pollution and high in yield, and is a novel industrial production method of the baclofen.

Description

technical field [0001] The invention relates to a method for producing GABA derivatives, in particular to a brand-new green industrial production method for baclofen, which belongs to the technical field of drug synthesis. Background technique [0002] With the various pressures that people face in life, changes in lifestyle, and factors such as age, various diseases such as stroke and its sequelae, cerebrovascular and its sequelae, gastroesophageal reflux disease, epilepsy, paralysis, etc. And so on unknowingly brought many serious harms to people. For example, the incidence of gastroesophageal reflux disease is increasing significantly, and the incidence among adults in western countries is about 10% to 30%. According to related reports, every 21 seconds in my country alone, one person dies of stroke. Stroke has become a common disease that endangers the lives of patients with cardiovascular and cerebrovascular diseases. At the same time, stroke can also cause sequelae su...

Claims

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Application Information

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IPC IPC(8): C07C227/04C07C229/34
CPCC07C227/04C07C51/09C07C67/343C07C231/14C07C253/30C07D211/88C07C229/34C07C233/11C07C57/58C07C69/65C07C255/41C07C255/35
Inventor 徐奎刘丽曽飞
Owner ANHUI YIXINMING PHARMA TECH
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