Process for the separation of 2-hydroxymethyl-3, 5-dimethyl-4-methoxy pyridine

A methoxypyridine and separation method technology, which is applied in the field of separation and purification of 2-hydroxymethyl-3, can solve problems such as difficult refining, affecting yield, increasing solubility, etc., to reduce environmental pollution, reduce production costs, and increase yield rate effect

Active Publication Date: 2011-01-19
ZHEJIANG HUAYI PHARMA CO LTD OF HANGZHOU HUADONG PHARMA GRP +1
View PDF0 Cites 2 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

During the synthesis of 2-hydroxymethyl-3,5-dimethyl-4-methoxypyridine, 2,3,5-collidine, 2,3,5-trimethyl-4-methoxy Oxypyridine, 2-formylmethyl-4-methoxy-3,5-lutidine, 2,3,5-trimethyl-4-hydroxypyridine and polymers and other impurities, impurities cause 2- The solubility of hydroxymethyl-3,5-dimethyl-4-methoxypyridine increases, and the crystallization cannot be completed, which obviously affects the yield, increases the production cost, precipitates more crystal impurities, and is difficult to refine

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
  • Process for the separation of 2-hydroxymethyl-3, 5-dimethyl-4-methoxy pyridine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] The method for separating and purifying 2-hydroxymethyl-3,5-dimethyl-4-methoxypyridine by molecular distillation, the proportion of high boiling point high polymer is about 10%, including the following steps:

[0027] (1) Molecular distillation to remove high-boiling-point polymer impurities: In the molecular distillation system, control the oil bath heating temperature to 150-250°C, vacuum degree ≤ 20mmHg, slowly add 500ml of 2-hydroxymethyl- 3,5-Dimethyl-4-methoxypyridine mother liquor was added at a speed of 10ml / min, and it took about 50 minutes to complete the addition, and the gas phase condensate was collected, about 450ml, and the distillation was stopped.

[0028] (2) Rectification to remove pyridine derivative impurities: In the rectification system of a 500ml three-necked flask and a φ20mm×800mm packed column, add 450ml of the easy-boiling liquid obtained by molecular distillation, separate by rectification under reduced pressure, and control the temperature o...

Embodiment 2

[0031] The method for separating and purifying 2-hydroxymethyl-3,5-dimethyl-4-methoxypyridine by scraper film distillation method, the proportion of high boiling point high polymer is about 10%, including the following steps:

[0032] (1) Scraper film distillation to remove high boiling point high polymer impurities: at 2m 2 In the scraper film distillation system, control the temperature of the oil bath at 180-220°C, the degree of vacuum ≤10mmHg, the speed of the scraper at 150 rpm, and slowly add the centrifugally separated 2-hydroxymethyl-3,5 at a rate of 200kg / h. - Dimethyl-4-methoxypyridine mother liquor 1000kg, add about 5h, collect and evaporate liquid, about 900kg, stop distillation;

[0033] (2) Rectification to remove impurities of pyridine derivatives: In the rectification system of a 1000L stainless steel tower kettle and a stainless steel screen rectification tower with a tower diameter of φ300×6000mm, add 900kg of 2-hydroxyl distilled from the scraped film distil...

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

PropertyMeasurementUnit
boiling pointaaaaaaaaaa
Login to view more

Abstract

The invention relates to a method for separating an intermediate of omeprazole, namely 2-hydroxymethyl-3, 5-dimethyl-4-methoxy pyridine. The method comprises the following steps of: distilling and removing high polymer impurities from a 2-hydroxymethyl-3, 5-dimethyl-4-methoxy pyridine mother solution containing pyridine derivative, high polymer and other impurities by an evaporator, and then separating and removing the pyridine derivative impurities from the mixed solution through a rectifying tower to separate a product. The product obtained by the method has the advantages of high purity, simple and convenient separation method, manufacturing cost reduction, environmental pollution reduction and suitability for industrial production.

Description

(1) Technical field: [0001] The present invention mainly relates to a method for separating and purifying 2-hydroxymethyl-3,5-dimethyl-4-methoxypyridine from a picoline mixture. (two) background technology: [0002] 2-Hydroxymethyl-3,5-dimethyl-4-methoxypyridine is a key intermediate of omeprazole, a proton pump inhibitor used to treat peptic ulcers. During the synthesis of 2-hydroxymethyl-3,5-dimethyl-4-methoxypyridine, 2,3,5-collidine, 2,3,5-trimethyl-4-methoxy Oxypyridine, 2-formylmethyl-4-methoxy-3,5-lutidine, 2,3,5-trimethyl-4-hydroxypyridine and polymers and other impurities, impurities cause 2- The solubility of hydroxymethyl-3,5-dimethyl-4-methoxypyridine increases, and the crystallization cannot be completed, which obviously affects the yield, increases the production cost, precipitates more crystal impurities, and is difficult to refine. (3) Contents of the invention: [0003] The task of the present invention is to overcome the shortcomings of completely relyi...

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
Patent Type & Authority Patents(China)
IPC IPC(8): C07D213/68
Inventor 王井明吴安生饶新堂廖新艳
Owner ZHEJIANG HUAYI PHARMA CO LTD OF HANGZHOU HUADONG PHARMA GRP
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