Check patentability & draft patents in minutes with Patsnap Eureka AI!

Preparation method of vitamin B6 intermediate

An intermediate and vitamin technology, applied in the field of preparation of vitamin B6 intermediate n-propyl dioxane, can solve the problems of increased processing difficulty, low raw material conversion rate, high boiling tar, etc., and achieve good catalytic effect and yield The effect of high efficiency and reduced production cost

Inactive Publication Date: 2013-03-13
HUAZHONG PHARMA
View PDF0 Cites 5 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method adopts the method of "one-pot cooking" feeding, the conversion rate of raw materials is low, and the reaction time is long, and it is easy to produce more high-boiling tar, which reduces the yield and increases the difficulty of handling in industrial production.

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Example 1 Preparation of n-propyldioxane

[0024] (1) Hemiacetal reaction:

[0025] a. Take each raw material according to the following ratios in parts by weight:

[0026] Cis-1,4-butenediol: 88 parts

[0027] Benzene: 44 parts

[0028] p-toluenesulfonic acid: 0.2 parts

[0029] Hydroquinone: 0.2 parts

[0030] N-butyraldehyde: 73 parts

[0031] b. Add cis-1,4-butenediol and benzene that meet the above ratio requirements into the reaction vessel, then dissolve the measured p-toluenesulfonic acid and hydroquinone in 1 part of pure water to make an aqueous solution Add the reaction system, add n-butyraldehyde dropwise at room temperature, and then keep the reaction at 50°C for 2h.

[0032] (2) Dehydration acetal reaction:

[0033] Connect the reflux water separation device, heat the above reaction solution under constant stirring, the reaction time is 2h, and separate 18 parts of water.

[0034] (3) Product distillation:

[0035] Connect the reflux device, conti...

Embodiment 2

[0037] Example 2 Preparation of n-propyldioxane

[0038] (1) Hemiacetal reaction:

[0039] a. Take each raw material according to the following ratios in parts by weight:

[0040] Cis-1,4-butenediol: 88 parts

[0041] Benzene: 44 parts

[0042] p-toluenesulfonic acid: 0.3 parts

[0043] Hydroquinone: 0.4 parts

[0044] N-butyraldehyde: 73 parts

[0045] b. Add cis-1,4-butenediol and benzene that meet the above ratio requirements into the reaction vessel, then dissolve the measured p-toluenesulfonic acid and hydroquinone in 1 part of pure water to make an aqueous solution Add the reaction system, add n-butyraldehyde dropwise at room temperature, and then keep the reaction at 50°C for 4h.

[0046] (2) Dehydration acetal reaction:

[0047] Connect the reflux water separation device, heat the above reaction solution under continuous stirring, the reaction time is 4 hours, and separate 18.5 parts of water.

[0048] Product distillation operating process is with embodiment 1...

Embodiment 3

[0050] Example 3 Preparation of n-propyldioxane

[0051] (1) Hemiacetal reaction:

[0052] a. Take each raw material according to the following ratios in parts by weight:

[0053] Cis-1,4-butenediol: 88 parts

[0054] Benzene: 44 parts

[0055] p-toluenesulfonic acid: 0.4 parts

[0056] Hydroquinone: 0.4 parts

[0057] N-butyraldehyde: 73 parts

[0058] b. Add cis-1,4-butenediol and benzene that meet the above ratio requirements into the reaction vessel, then dissolve the measured p-toluenesulfonic acid and hydroquinone in 1 part of pure water to make an aqueous solution Add the reaction system, add n-butyraldehyde dropwise at room temperature, and then keep the reaction at 50°C for 4h.

[0059] (2) Dehydration acetal reaction:

[0060] Connect the reflux water separator, heat the above-mentioned reaction solution under continuous stirring, the reaction time is 6 hours, and separate 19 parts of water.

[0061] Product distillation operating process is with embodiment 1...

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 relates to a preparation method of a vitamin B6 intermediate n-propyl dioxepin. The preparation method is characterized in that benzene is used as a solvent, in the presence of p-toluenesulfonic acid and hydroquinone, n-butanal is reacted with cis-1, 4-butylene glycol to get the intermediate n-propyl dioxepin of the vitamin B6. The catalyst used in the method is excellent in reaction activity and can simultaneously inhibit the intramolecular dehydration and aggregation of the cis-1, 4-butylene glycol, and the catalyst is added in a water solution form, is dispersed uniformly, is excellent in catalytic effect, and generates less in side reaction and high boiling in distillation, so that the production cost is lowered greatly.

Description

technical field [0001] The present invention relates to a preparation method of a pharmaceutical intermediate, in particular to a vitamin B 6 Preparation method of intermediate n-propyldioxane. Background technique [0002] N-propyldioxane, the chemical name is 2-n-propyl-4,7-dihydro-1,3-dioxepepin, it is synthesized vitamin B by oxazole method 6 intermediate raw materials. Vitamin B 6 It participates in the metabolism of amino acids and proteins in the organism, and plays a vital role in the treatment of pregnancy vomiting, drug-induced gastrointestinal reactions, and the prevention of toxic and side effects of anti-tuberculosis isoniazid and other diseases. In addition to being used for medicine, vitamin B 6 It also plays an important role in nutrition and health care during the metabolism of livestock and poultry, thus becoming a necessary feed additive in the modern feed industry, and is widely used in the preparation of complete feed. It is also used to fortify foo...

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 Applications(China)
IPC IPC(8): C07D321/06
Inventor 王勇李新宇付林徐勇李小平
Owner HUAZHONG PHARMA
Features
  • R&D
  • Intellectual Property
  • Life Sciences
  • Materials
  • Tech Scout
Why Patsnap Eureka
  • Unparalleled Data Quality
  • Higher Quality Content
  • 60% Fewer Hallucinations
Social media
Patsnap Eureka Blog
Learn More

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

© 2025 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com