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Photochemical method for synthesizing vitamine D3

A technology for photochemical synthesis and vitamins, which is applied in organic chemistry and other fields, can solve the problems of large-scale production difficulties, troublesome post-processing, and difficulty in realizing industrialization, and achieve the effects of increased yield, simple production process, and increased concentration of reactants

Inactive Publication Date: 2003-10-01
TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The illumination systems involved in these studies are complicated, post-processing troubles, and difficult to realize industrialization (Kobayashi, T.; Yasumura, M.J.Nutr.Sci.Vitaminol., 1973, 19, 123-128; Sato, T.; Yamauchi, H.; Ogata , Y., Kunii, T.; Kagei, K.; Katsui, G.; Toyoshima, S.; Yasumura, M.; Kobayashi, T. J. Nutr. Sci. Vitaminol., 1980, 26, 545-556; ; Phillips, R.B. J.Am.Chem.Soc., 1982, 104, 355-356; Dauben, W.G.; Phillips, R.B., J.Am.Chem.Soc., 1982, 104, 5780-5781)
In addition, 7-dehydrocholesterol has oil-water amphiphilicity, and its solubility in common solvents at room temperature does not exceed 1%, which makes it difficult for large-scale production

Method used

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  • Photochemical method for synthesizing vitamine D3
  • Photochemical method for synthesizing vitamine D3
  • Photochemical method for synthesizing vitamine D3

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] (1). Light reaction of 7-dehydrocholesterol

[0033] In a 500 ml round bottom flask, 16.5 g of 7-dehydrocholesterol was dissolved in 330 ml of petroleum ether (30-60°C)-ethanol (6:1, V / V) mixed solvent, and 10 mg of 2,6- Di-tert-butyl-p-methoxyphenol is uniformly mixed with magnetic stirring to prepare a photochemical reaction solution. The reaction solution was placed in a 450-watt high-pressure mercury lamp (Beijing Electric Light Source Research Institute GGZ1000-1) and an in-immersion photochemical reactor that was being ventilated with nitrogen. Adjust the nitrogen flow rate to make the bubbles uniform. Start the mercury lamp and time it. The reaction device is placed in a light-tight fume hood, and an electric fan is added to ensure that the temperature of the photochemical reaction solution does not exceed 28°C, so as to avoid premature formation of vitamin D during the photochemical reaction. 3 . The reaction was monitored by high pressure liquid chromatogra...

Embodiment 2

[0041] (1). Light reaction of 7-dehydrocholesterol

[0042] In a 500 ml round bottom flask, 16.5 g of 7-dehydrocholesterol was dissolved in 330 ml of pentane-methanol (6:1, V / V) mixed solvent, and 10 mg of 2,6-di-tert-butyl-p- Methoxyphenol, mixed evenly with a magnetic stirrer, and configured as a photochemical reaction solution. The reaction solution was placed into a 450-watt high-pressure mercury lamp (same as in Example 1) and in an in-immersion photochemical reactor that was being ventilated with nitrogen. Adjust the nitrogen flow rate to make the bubbles uniform. Start the mercury lamp and time it. The reaction device is placed in a light-tight fume hood, and an electric fan is added to ensure that the temperature of the photochemical reaction solution does not exceed 28°C, so as to avoid premature formation of vitamin D during the photochemical reaction. 3 . The reaction was monitored by high pressure liquid chromatography (HPLC) (conditions were the same as in Exa...

Embodiment 3

[0050] (1). Light reaction of 7-dehydrocholesterol

[0051] In a 500 ml round bottom flask, dissolve 16.5 g of 7-dehydrocholesterol in 330 ml of hexane-dioxane (6:1, V / V) mixed solvent, add 10 mg of 2,6-di-tert-butyl Base-p-methoxyphenol, mixed evenly with magnetic stirring, and configured as a photochemical reaction solution. The reaction solution was placed into a 450-watt high-pressure mercury lamp (same as in Example 1) and in an in-immersion photochemical reactor that was being ventilated with nitrogen. Adjust the nitrogen flow rate to make the bubbles uniform. Start the mercury lamp and time it. The reaction device is placed in a light-tight fume hood, and an electric fan is added to ensure that the temperature of the photochemical reaction solution does not exceed 28°C, so as to avoid premature formation of vitamin D during the photochemical reaction. 3 . The reaction was monitored by high pressure liquid chromatography (HPLC) (conditions were the same as in Example...

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Abstract

A photochemical process for synthesizing VD3 includes such steps as dissolving 7-dehydrocholesterol in the mixture of polar solvent and non-polar solvent, adding antioxidizing agent, stirring, light radiating at 23-30 deg.C, evaporating, adding polar solvent, separating the unreacted 7-dehydrocholesterol, adding maleic acid anhydride and aqueous solution of KOH or NaOH while stirring to obtain viscose material, dissolving in refined oil, vacuum heating to 60-70 deg.C and vacuum relief. Its advantage is high output rate about 70%.

Description

technical field [0001] The invention belongs to the field of organic photochemical synthesis, in particular to photochemical synthesis of vitamin D 3 Methods. Background technique [0002] Vitamin D 3 It is one of the important vitamins essential for human health, normal growth and reproduction of livestock and poultry, and it needs to be added in an appropriate amount in food and feed. With the development of society and the improvement of people's living standards, vitamin D 3 It has a wide range of markets at home and abroad. At present, only a few countries such as Germany and Switzerland produce it in the world, and the price is expensive. Chinese manufacturers have used dozens of one-kilowatt mercury lamps as the light source, ethanol as the solvent, the photochemical reaction temperature is above 60°C, the concentration of the reaction raw materials is not more than 2%, the conversion rate is 100%, and there are many by-products. Product pu...

Claims

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Application Information

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IPC IPC(8): C07C401/00
Inventor 张宝文程学新刘颙颙王雪松曹怡
Owner TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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