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A kind of preparation method of vitamin B6

A vitamin and methyl technology, which is applied in the field of preparation of high-content vitamin B6, can solve the problems that the content of vitamin B is difficult to meet the medicinal standard, it is difficult to completely remove by-products, and the color of the product is heavy, so as to avoid multiple recrystallization and decolorization The effect of operation, high product yield and thorough reaction

Active Publication Date: 2021-01-22
XINFA PHARMA
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Among them, deethanol aromatization requires relatively high acidity of the reaction system, which leads to the rearrangement of Diels-Alder addition products to generate pyrroles and bimolecular dehydration by-products, which makes the product more heavily colored and makes decolorization difficult. Even if it is adsorbed many times, it is also difficult. Completely remove the pyrroles and bimolecular dehydration by-products, resulting in vitamin B 6 Difficult to reach pharmaceutical standards

Method used

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  • A kind of preparation method of vitamin B6
  • A kind of preparation method of vitamin B6
  • A kind of preparation method of vitamin B6

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Example 1: 1,5-dihydro-3-n-propyl-8-methyl-9-methylcarbonyloxypyrido[3,4-e]-1,3-dioxane (V1) preparation of

[0035] Add 63.5 g (0.5 mol) of 4-methyl-5-ethoxyoxazole, 285.0 g (2.0 mol) of 2-n-propyl-4,7-dihydro-1,3- Dioxheptin, 60 g (0.6 moles) of acetic anhydride, replaced by nitrogen three times, heated to an internal temperature of 135-145° C., stirred for 8 hours, and the reaction pressure was 0.2-0.3 MPa. Lower the temperature to 50-60°C, and recover by-product ethanol, acetic acid, a small amount of acetic anhydride and excess 2-n-propyl-4,7-dihydro-1,3-dioxepin (separated by rectification) After ethanol and acetic acid, it can be used directly), and the product was collected by distillation at 160-180°C / 2-3mmHg under high vacuum to obtain 129.2 grams of 1,5-dihydro-3-n-propyl-8-methyl-9-methanol Carbonyloxypyrido[3,4-e]-1,3-dioxane (V1), yield 97.5%, HPLC purity 99.9%.

Embodiment 2

[0036] Example 2: 1,5-dihydro-3-n-propyl-8-methyl-9-methylcarbonyloxypyrido[3,4-e]-1,3-dioxane (V1) preparation of

[0037] Add 56.5 g (0.5 mol) of 4-methyl-5-methoxyoxazole, 285.0 g (2.0 mol) of 2-n-propyl-4,7-dihydro-1,3- Dioxheptin, 71.5 g (0.7 moles) of acetic anhydride, replaced by nitrogen three times, heated to an internal temperature of 130-135° C., stirred for 12 hours, and the reaction pressure was 0.3-0.4 MPa. Lower the temperature to 50-60°C, and recover by-product methanol, acetic acid, a small amount of acetic anhydride and excess 2-n-propyl-4,7-dihydro-1,3-dioxepin by distillation under reduced pressure (separated by rectification Methanol and acetic acid can be used directly), and the product was collected by distillation under high vacuum (160-180°C / 2-3mmHg) to obtain 129.0 g of 1,5-dihydro-3-n-propyl-8-methyl-9 -Methylcarbonyloxypyrido[3,4-e]-1,3-dioxane (V1), yield 97.4%, HPLC purity 99.9%.

Embodiment 3

[0038] Example 3: 1,5-dihydro-3-n-propyl-8-methyl-9-methylcarbonyloxypyrido[3,4-e]-1,3-dioxane (V1) preparation of

[0039] Add 63.5 g (0.5 mol) of 4-methyl-5-ethoxyoxazole, 142.5 g (1.0 mol) of 2-n-propyl-4,7-dihydro-1,3- Dioxheptin, 60.0 g (0.6 moles) of acetic anhydride, replaced with nitrogen three times, heated to an internal temperature of 135-145° C., stirred for 9 hours, and the reaction pressure was 0.2-0.3 MPa. Cool down to 50-60°C, and recover by-product ethanol, acetic acid, a small amount of acetic anhydride, unreacted 4-methyl-5-ethoxyoxazole, 2-n-propyl-4,7-dihydro by vacuum distillation -1,3-Dioxheptin (can be used directly after separation of ethanol and acetic acid by rectification), the product was collected by distillation at 160-180℃ / 2-3mmHg under high vacuum to obtain 86.8 grams of 1,5-dihydro- 3-n-propyl-8-methyl-9-methylcarbonyloxypyrido[3,4-e]-1,3-dioxane (V1), yield 95.5% (based on the actual consumption of 4 -methyl-5-ethoxyoxazole), the HPLC puri...

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Abstract

The invention relates to a preparation method of a high content vitamin B6. According to the method, 1,5-dihydro-3,3-disubstituent group-8-methyl-9-alkyl carbonyl oxypyrido [3,4-e]-1,3-dioxane is prepared by the Diels-Alder addition reaction, aromatization reaction and esterification reaction of 4-methyl-5-alkoxyl-oxazole and 2,2-disubstituent group-4,7-dihydro-1,3-dioxepine in the presence of ananhydride through the "one-pot method", and then vitamin B6 is prepared by deprotection. According to the method, the stability of the raw materials of 4-methyl-5-alkoxyl-oxazole and 2,2-disubstituentgroup-4,7-dihydro-1,3-dioxepine are ensured, the reaction is thorough, and the selectivity is high, so that the method provides guarantees for the preparation of high content medicinal vitamin B6.

Description

technical field [0001] The invention relates to a high-content vitamin B 6 The preparation method belongs to the technical field of pharmaceutical biochemical industry. Background technique [0002] Vitamin B 6 (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. 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. [0003] At present, the industry usually uses chemical synthesis to produce vitamin B 6 , Chinese patent documents CN101402600A and CN102329048A use 4-methyl-5-ethoxyoxazole and 2-n-propyl-4,7-dihydro-1,3-dioxin through Diels-Alder addition reaction, Deethanol aromatization, hydrolysis to remove n-butyraldeh...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D213/67C07D491/056
CPCC07D213/67C07D491/056
Inventor 戚聿新李新发吕强三王成威鞠立柱
Owner XINFA PHARMA
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