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Simple preparation method of vitamin B6

A vitamin and simple technology, applied in the field of medicine and biochemical industry, can solve the problems of environmental pollution, long production cycle, heavy product coloring, etc., and achieve the effect of shortening the process cycle, short reaction cycle, simple operation and environmental protection.

Active Publication Date: 2015-07-15
XINFA PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, the existing VB 6 The chemical synthesis method of the preparation process mostly includes addition reaction and aromatization reaction, etc., and there are problems such as long production cycle, many three wastes generated, environmental pollution, and the product is heavily colored and difficult to decolorize.

Method used

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  • Simple preparation method of vitamin B6
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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Example 1: Preparation of 5-formyl-6-cyano-1,3-dioxepane

[0042] Add 200 grams of methanol, 83 grams (1.0 mole) of 3-cyanopropanal, 350 grams (3.5 moles) of 30% formaldehyde solution, 12 grams of zinc chloride, 15 grams of 30% hydrochloric acid, and nitrogen replacement in a 1000 milliliter reactor The second time, the temperature was raised to 80°C for 7 hours (the pressure was 2 atmospheres). Methanol was recovered, cooled, extracted three times with ethyl acetate (a total of 460 g was used), and the solvent was recovered to obtain 146.2 g of 5-formyl-6-cyano-1,3-dioxepane with a purity of 98.7% (GC). Yield 94.3%.

Embodiment 2

[0043] Example 2: Preparation of 5-formyl-6-cyano-1,3-dioxepane

[0044] Add 200 grams of 95% ethanol, 83 grams (1.0 moles) of 3-cyanopropionaldehyde, 350 grams (3.5 moles) of 30% formaldehyde solution, 15 grams of zinc chloride dihydrate, and 15 grams of 30% hydrochloric acid in a 1000 milliliter reactor , replaced with nitrogen three times, and heated to 80°C for 7 hours (pressure about 1.8 atmospheres). Methanol was recovered, cooled, extracted three times with ethyl acetate (500 g in total), and the solvent was recovered to obtain 145.4 g of 5-formyl-6-cyano-1,3-dioxepane with a purity of 98.3% (GC). The yield is 93.8%.

Embodiment 3

[0045] Example 3: Preparation of 5-formyl-6-cyano-1,3-dioxepane

[0046] Add 200 grams of methanol, 83 grams (1.0 moles) of 3-cyanopropanal, 350 grams (3.5 moles) of 30% formaldehyde solution, 12 grams of zinc acetate dihydrate, 15 grams of 30% hydrochloric acid, and replace with nitrogen in a 1000 ml reactor 3 times, the temperature was raised to 80°C for 7 hours (the pressure was 2 atmospheres). Methanol was recovered, cooled, extracted three times with ethyl acetate (a total of 450 g was used), and the solvent was recovered to obtain 143.4 g of 5-formyl-6-cyano-1,3-dioxepane with a purity of 98.9% (GC). Yield 92.5%.

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Abstract

The invention relates to a simple preparation method of vitamin B6. The method comprises the following steps: getting 2-aminopropionic ester hydrochloride and 3-formylpropiononitrile as starting materials; enabling the 3-formylpropiononitrile and formaldehyde to react at a temperature of 30 to 100 DEG C under the effect of an acid catalyst to obtain 5-formoxyl-6-cyan-1 and 3-dioxo cycloheptane; and then synthesizing the vitamin B6 through ring formation and hydrolysis reaction. The simple preparation method of vitamin B6 has the advantages that a 4-methyl-5-alkoxy oxazole intermediate which is difficult to prepare is not used, and diels-Alder addition reaction needing high temperature is removed, thus the process cycle is shortened, the operation is simple, the environmental protection is realized, and the cost is low; in addition, the reaction selectivity is high, and the vitamin B6 has high purity; the simple preparation method of vitamin B6 is more suitable for scale industrial production.

Description

technical field [0001] The invention relates to a simple method for preparing vitamin B 6 The method belongs to the field of pharmaceutical biochemical technology. Background technique [0002] Vitamin B 6 It is one of the essential vitamins for the human body and plays a key role in the growth of animals, so it is widely used in the fields of medicine, food, feed additives and cosmetics industries. Vitamin B 6 (referred to as VB 6 ) exists in nature in three forms: pyridoxine, pyridoxal and pyridoxamine. Under certain conditions, the three can be transformed into each other in vivo. Industrial synthesis is generally pyridoxine hydrochloride. At present, the industry usually uses chemical synthesis to produce vitamin B 6 , as mentioned in U.S. Patent US3227721, 2-methyl-3-hydroxy-pyridine-4,5-dicarboxylic acid diethyl ester uses lithium tetrahydrogen as a reducing agent to prepare vitamin B 6 , but the amount of lithium tetrahydrogen is large, the price is expensive,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D213/67
CPCC07D213/67
Inventor 戚聿新李新发吕强三鞠立柱
Owner XINFA PHARMA
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