Method for recovering galantamine intermediate raw material 2-bromo-5-hydroxy-4-methoxybenzoic acid

A technology of methoxybenzoic acid and galantamine, applied in the field of biomedicine, can solve the problems of high cost of production materials and high cost of three-waste treatment, and achieve the effect of reducing waste water

Pending Publication Date: 2021-08-24
SCINOPHARM CHANGSHU PHARMA
View PDF6 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The auxiliary raw material B13 is excessive, the cost of production materials is high, and the cost of three wastes is also high

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Method for recovering galantamine intermediate raw material 2-bromo-5-hydroxy-4-methoxybenzoic acid
  • Method for recovering galantamine intermediate raw material 2-bromo-5-hydroxy-4-methoxybenzoic acid
  • Method for recovering galantamine intermediate raw material 2-bromo-5-hydroxy-4-methoxybenzoic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0074] Step 1: Add soft water and sodium hydroxide to the RX-2102 reaction kettle, stir until the sodium hydroxide solution is completely dissolved, and transfer the sodium hydroxide solution to the bucket for use; the concentration of the sodium hydroxide solution is 20%.

[0075] Step 2: Under nitrogen, add soft water and 36% hydrochloric acid into the RX-2105 reactor, stir for ≥ 10 minutes to obtain a hydrochloric acid solution, and transfer the hydrochloric acid solution to a barrel for use; the concentration of the hydrochloric acid solution is 15%.

[0076] Step 3: Under nitrogen condition, add the B13-OMe to be recovered into the RX-2102 reactor, and take a sample to detect that the B13-OMe content is 11%.

[0077] Step 4: Distill the contents of the RX-2102 reactor to 1 times, and the inner temperature of the RX-2102 reactor is 21°C.

[0078] Step 5: Under nitrogen, add the sodium hydroxide solution into the RX-2102 reaction kettle, and control the internal temperatur...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

Abstract

The invention discloses a method for recovering a galantamine intermediate raw material 2-bromine-5-hydroxy-4-methoxybenzoic acid, wherein the method comprises the following scheme: layering a mixed solution of dichloromethane and water in a waste liquid, distilling and reducing a water layer, and carrying out outsourcing incineration on distillation residues as the waste liquid; and distilling out most of a solvent from a dichloromethane layer, reusing the solvent as a recovery solvent in an original galantamine intermediate process, adding a sodium hydroxide aqueous solution into distillation residues, hydrolyzing and reducing into B13, adjusting the pH value of the solution after the reaction is finished, separating out a solid to obtain a crude product B13, and carrying out a primary purification process to obtain the high-quality B13. B13-OMe is effectively reduced into B13, mother liquor is subjected to classified treatment, and the waste treatment cost is reduced.

Description

technical field [0001] The invention relates to the field of biomedicine, in particular to a method for recovering 2-bromo-5-hydroxy-4-methoxybenzoic acid, a galantamine intermediate raw material. Background technique [0002] In the original Galantamine (Galantamine) intermediate process, the amount of auxiliary raw material B13 used is 375Kg / batch, and the equivalent number with the main raw material is 1.4:1. After batch production, B13-OMe (2-bromo-5- The state of hydroxy-4-methoxybenzoic acid methyl ester) is dissolved in the mother liquor, and is used as waste liquid to be incinerated outside. [0003] The auxiliary raw material B13 is excessive, the cost of production materials is high, and the cost of three wastes is also high. Contents of the invention [0004] In order to overcome the defects in the prior art, the embodiment of the present invention provides a method for recovering 2-bromo-5-hydroxyl-4-methoxybenzoic acid, an intermediate raw material of galanta...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
IPC IPC(8): C07C65/21C07C51/09C07C51/42C07C51/44
CPCC07C51/09C07C51/42C07C51/44C07C65/21
Inventor 肖俊韦秀琼
Owner SCINOPHARM CHANGSHU PHARMA
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap