Preparation method of 6-aminocaproic acid

A technology of aminocaproic acid and dilute sulfuric acid is applied in the preparation of organic compounds, chemical instruments and methods, and cyanide reaction preparation, etc., to achieve the effects of convenient operation, simple reaction conditions, and high production cost reduction.

Pending Publication Date: 2018-09-18
CHANGZHOU LANLING PHARMA
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0017] The purpose of the present invention is to solve the shortcomings of the existing caprolactam hydrolysis method, to provide a 6-aminocaprolactam hydrolysis method with convenient operation, simple reaction conditions, low production cost, low environmental pollution, high yield, and suitable for large-scale industrial production. acid preparation method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1）

[0030] The preparation method of the 6-aminocaproic acid of the present embodiment has the following steps:

[0031] ① Add 198g of caprolactam (1.75mol), 88g of sodium hydroxide (2.2mol) and 1000g of demineralized water into a 2L reaction flask, raise the temperature to 103°C, and carry out the alkaline hydrolysis reaction for 1.5h.

[0032] ② Cool the material after alkaline hydrolysis in step ① to room temperature, and neutralize it with dilute sulfuric acid with a concentration of 15wt% to pH=7.5.

[0033] ③The material after the neutralization treatment in step ② is added to the electrodialysis device for desalination treatment, and the sulfate radical content in the effluent is less than 100ppm as the end point.

[0034] ④ Decolorize the desalted material in step ③ with activated carbon, filter it, concentrate the filtrate at 47-70°C to near-dryness, add ethanol while it is hot, stir and crystallize, cool, and filter to obtain crude 6-aminocaproic acid.

[0035] Then dis...

Embodiment 2～ Embodiment 5）

[0037] The preparation method of each embodiment is basically the same as that of Example 1, and the differences are shown in Table 1.

[0038] Table 1

[0039]

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PUM

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Abstract

The invention discloses a preparation method of 6-aminocaproic acid. The 6-aminocaproic acid is obtained by using caprolactam as a raw material through alkali hydrolysis, neutralization processing, desalination processing and refining processing; alkali hydrolysis is that the caprolactam reacts with sodium hydroxide and water for 1 to 5h at a temperature of 100 to 110 DEG C; neutralization processing is that the material obtained after alkali hydrolysis is cooled to room temperature and is neutralized into pH of 7.5 by dilute sulphuric acid; desalination processing is that the material obtained after neutralization processing is subjected to desalination of electrodialysis. According to the method disclosed by the invention, an alkali hydrolysis method is adopted, then the dilute sulphuricacid is adopted to neutralize the material obtained after alkali hydrolysis into an isoelectric point of the 6-aminocaproic acid, and electrodialysis is utilized to desalinate. The method not only isconvenient to operate and simple in reaction condition, but also does not need to adopt ion exchange resin so as to greatly reduce the defects of higher production cost, serious pollution to the environment and the like of a resin absorption method; particularly, the method is higher in yield, is basically 95% or more and is suitable for industrial mass production.

Description

technical field [0001] The invention belongs to the technical field of medicine preparation, and in particular relates to a preparation method of a hemostatic drug 6-aminocaproic acid. Background technique [0002] 6-Aminocaproic acid (6-Aminocaproic Acid) is an antifibrinolytic drug. Fibrinogen specifically binds to fibrin through the lysine binding site in its molecular structure, and then becomes plasmin under the action of an activator, which can cleave the arginine and lysine peptide chains in fibrin , forming fibrin degradation products that dissolve blood clots. This product can inhibit the combination of plasminogen and fibrin, prevent its activation, thereby inhibiting fibrinolysis, high concentration can directly inhibit the activity of plasmin, and achieve hemostatic effect. [0003] At present, the preparation method of 6-aminocaproic acid mainly contains the following kinds: [0004] 1. Chemical synthesis method: refer to Chinese patent document CN1505606A. ...

Claims

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Application Information

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IPC IPC(8): C07C227/22C07C227/40C07C229/08
CPCC07C227/22C07C227/40C07C229/08
Inventor 虞小平徐永明吴小波
Owner CHANGZHOU LANLING PHARMA
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