Photochemical synthesis preparation method for vitamin D2

A technology of photochemical synthesis and vitamins, applied in the direction of organic chemistry, etc., can solve the problems of poor production technology, affecting cost and output, and difficult industrial production of vitamin D, and achieve the effect of low production cost and simple production process

Active Publication Date: 2006-05-03
SICHUAN NEIJIANG HUIXIN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Vitamin D adopted by Chinese enterprises 2 The production process is poor, and the yield is only about 20%, which is only 2 / 3 of the yield level in developed countries, thus affecting the cost and output
[0003] Chinese patent (ZL87101241) discloses a method for laser synthesis of vitamin D, which alternately irradiates with lasers of two wavelengths to synthesize pre-vitamin D through photochemical isomerization, and then generates vitamin D through thermal isomerization, but due to the low efficiency of using laser, It has not been practically applied to industrial scale production at present
[0006] The purpose of the present invention is to be difficult to realize industrialized production vitamin D for above-mentioned existing technology complexity 2 situation, using commonly used chemical equipment and raw materials to achieve industrial production of vitamin D 2 The goal

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] (1) Photoirradiation reaction of ergosterol

[0020] Put 5 kg of ergosterol and 750 L of ethanol (concentration ≥ 90%, temperature 60° C.) into a dissolving pot for dissolution to form a photoreaction solution. The light reaction solution enters the irradiator through the flowmeter, and is illuminated with ultraviolet light from a low-pressure (220V) mercury lamp, then concentrated in a concentrator under reduced pressure to remove ethanol and crystallization to filter out unconverted ergosterol, and the obtained filtrate is pumped into a Kjeldahl distillation flask Nitrogen gas (flow rate 2L / min) was introduced, and the concentration was continued. Orange-yellow resinous vitamin D 2 Crude conversion oil.

[0021] (2) Chromatography

[0022] Vitamin D 2 Crude converted oil is dissolved in benzene (volume ratio is 1:6), and then flows through the chromatographic tube equipped with alumina, concentrated under reduced pressure in the concentration pot to remove benzene...

Embodiment 2

[0028] (1) Photoirradiation reaction of ergosterol

[0029] Take 5kg of angular sterol and 1500L ethanol (concentration ≥ 94%, temperature 70°C) and put them into a dissolving pot for dissolution to form a photoreaction solution. Illumination, then concentrated under reduced pressure in a concentration pot to remove ethanol and crystallization to filter out unconverted ergosterol, the resulting filtrate was pumped into a Kjeldahl distillation flask and fed with nitrogen (flow rate 5L / min), and then continued to concentrate to obtain orange-yellow resinous vitamin D. 2 Crude converted oil;

[0030] (2) Chromatography

[0031] Vitamin D 2 Crude converted oil is dissolved in benzene (volume ratio 1:13), then flows through a chromatographic tube equipped with alumina, is concentrated under reduced pressure in a concentrating pot to remove benzene, is then pumped into a Kjeldahl distillation flask and fed with nitrogen, and then continues Concentrate to get orange-yellow resino...

Embodiment 3

[0037] (1) Photoirradiation reaction of ergosterol

[0038] Take 5kg of ergosterol and 1300L ethanol (concentration ≥ 94%, temperature 66°C) into a dissolving pot for dissolution to form a photoreaction solution. The photoreaction solution enters the irradiator through a flowmeter, and is processed by a low-pressure (220V) mercury lamp with ultraviolet rays. Illuminated, then concentrated under reduced pressure in a concentration pot to remove ethanol and crystallized to filter off unconverted ergosterol, and the resulting filtrate was sucked into a Kjeldahl distillation flask and fed with nitrogen (flow rate 4L / min) and then concentrated. Orange-yellow resinous vitamin D 2 Crude converted oil;

[0039] (2) Chromatography

[0040] Vitamin D 2 The crude converted oil is dissolved in benzene (volume ratio is 1:10), then flows through the chromatographic tube equipped with alumina, is concentrated under reduced pressure in a concentrating pot to remove benzene, is then pumped ...

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PUM

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Abstract

The invention relates to preparation method for vitamin D2 by actinochemical way, which comprises: preparing photoreaction liquid with ergosterin and ethanol, irradiating with ultraviolet ray from low-pressure mercury vapor lamp to obtain the D2 coarse product; after chromatography, esterification and hydrolysis, drying to obtain the product. This invention realizes the industrial product with simple process and low cost.

Description

technical field [0001] The present invention relates to vitamin D 2 field, in particular to the field of water-soluble vitamin D2 preparation method. Background technique [0002] Vitamin D 2 It is one of the trace organic compounds necessary for humans and animals to maintain normal life activities and health. Vitamin D can be added in moderation in medicines, food and feed 2 To meet the regular intake of people or animals from the outside world. Vitamin D 2 is the main natural form of vitamin D found in plants. (referring to Chinese patent 95118188.27. And vitamin is divided into two classes namely fat-soluble vitamin (A, D, E, K) etc. according to its solubility, or water-soluble vitamin (B 1 , B 2 , B 6 , B 1 ), folic acid, niacin and vitamin C), etc. [See Chapter 15 of "Medicinal Chemistry", 1. The classification of vitamins (Wang Shuxia, Department of Agriculture and Medicine, Central TV University)]. due to vitamin D 2 It is insoluble in water but soluble i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C401/00
Inventor 陈国苹
Owner SICHUAN NEIJIANG HUIXIN PHARMA
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