Unlock instant, AI-driven research and patent intelligence for your innovation.

Preparation method of high-purity vitamin B6

A vitamin and aromatization technology, which is applied in the field of chemical synthesis of vitamins, can solve the problems of increasing operation steps, solidifying waste with activated carbon, and consuming large amounts of energy, and achieves the effects of simplified steps, high recovery rate and energy saving.

Pending Publication Date: 2022-04-12
XINFA PHARMA
View PDF4 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the refining steps in the existing technology, the crude vitamin B6 needs to go through multiple times of activated carbon decolorization and multiple times of water recrystallization, so that the final product can approach food-grade and pharmaceutical-grade standards; this process consumes a lot of pure water, and the temperature of the hot water is at 80°C Left and right, heating water needs to consume a lot of energy, generate a lot of waste water, generate a lot of activated carbon solid waste, pollute the environment, and increase the operation steps, resulting in an increase in overall costs

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
  • Preparation method of high-purity vitamin B6
  • Preparation method of high-purity vitamin B6
  • Preparation method of high-purity vitamin B6

Examples

Experimental program
Comparison scheme
Effect test

preparation example 1

[0100] Preparation Example 1: Diels-Alder Reaction

[0101] The Diels-Alder reaction product of the present invention can be prepared according to the prior art. For example, it can be prepared according to the following method: add 800g of compound 2 into a reaction flask and heat up to 150°C, then add 75g of compound 1, keep it in the temperature range of 140-160°C for 10-15 hours, and then distill under reduced pressure until there is basically no distillation. The compound 3 was obtained.

Embodiment 1

[0102] Embodiment 1: aromatization reaction

[0103] Add 180mL of 95wt% ethanol aqueous solution to 300g of compound 3 of reaction formula D, replace with nitrogen, control the temperature at 25-30°C, and add 200ml of 0.2mol / L hydrochloric acid aqueous solution dropwise under stirring conditions, and control the temperature at 25-30°C after dropping , stirring and reacting for 12 hours; distill ethanol under reduced pressure at 50°C until the system is viscous, add 300ml of dichloromethane, stir and mix evenly, cool down to 5°C, and grow crystals for 1h. Suction filtration, rinse with dichloromethane; 229 g of compound 4 crystals were obtained for later use. The molar yield of the aromatization reaction was 92%.

Embodiment 2

[0104] Embodiment 2: the preparation of vitamin B6 crude product (hydrolysis reaction)

[0105] Add 800ml of dichloromethane and 229g of the compound 4 prepared in Example 1 into the reaction flask, add 130ml of 32wt% concentrated hydrochloric acid, and reflux under normal pressure at about 40°C for 3h under stirring conditions, add a water separator to the reflux device, and discharge the water from the reaction system. The organic phase was returned to the reaction bottle, refluxed to divide the water until the reaction was completed; the temperature was lowered to 5°C, the crystal was grown for 1 hour, filtered, the filter cake was washed with 95wt% ethanol aqueous solution, and vacuum-dried at 40-70°C to obtain crude vitamin B6, 207g. The molar yield of the hydrolysis reaction is 98%.

[0106] figure 1 The obtained vitamin B6 crude product purity, content, impurity A content, HPLC chart; Vitamin B6 crude product (H029-S) purity 99.88%, impurity A (H029-S-I-06) content 0.0...

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 provides a preparation method of high-purity vitamin B6. According to the method disclosed by the invention, the refined vitamin B6 is obtained through the steps of aromatization reaction, hydrolysis reaction and refining. According to the method disclosed by the invention, the aromatization reaction, the hydrolysis reaction and the refining step are subjected to process improvement, and particularly, an organic solvent is added into a reaction system in the hydrolysis reaction step, so that the method has a prominent effect on improvement of the preparation process of the vitamin B6. The method disclosed by the invention has the advantages of high product purity, high content, few impurities, light color, high yield, simplicity and convenience in operation, energy conservation, low cost and reduction of emission of three wastes.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis of vitamins, and in particular relates to a preparation method of high-purity vitamin B6. Background technique [0002] The main commercial form of vitamin B6, pyridoxine hydrochloride, is widely used in feed additives, food additives, health products, medicines and other fields. [0003] At present, the industry generally adopts the oxazole method to synthesize vitamin B6. In the method, refined vitamin B6 is obtained through Diels-Alder (Diels-Alder) reaction, aromatization reaction, hydrolysis reaction and refining steps. [0004] The existing report of adopting the oxazole method to synthesize vitamin B6 is as follows: [0005] Patent literature CN101402600A discloses a preparation method of vitamin B6, which adds an alkaline reagent (triethylamine) to the Diels-Alder reaction, and the aromatization reaction system is Diels-Alder reaction product, ethanol, water, hydrochloric acid...

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): C07D213/67
Inventor 李新发孔瑜王成威吴柯刘宁宁
Owner XINFA PHARMA