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 pro

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