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Photochemical method for synthesizing vitamine D3

A technology for photochemical synthesis and vitamins, applied in the direction of organic chemistry, etc., can solve the problems of difficulty in mass production, troublesome post-processing, and difficulty in realizing industrialization, and achieve the effect of improving yield, simple production process, and increasing the concentration of reactants.

Inactive Publication Date: 2005-04-13
TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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  • Abstract
  • Description
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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

[0031] (1) Light response of 7-dehydrocholesterol

[0032] 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 internal immersion photochemical reactor that was vented with nitrogen. Adjust the flow of nitrogen to make the bubbles uniform. Start the mercury lamp and count it. The reaction device is placed in an opaque fume hood, and an electric fan is added to ensure that the temperature of the photochemical reaction solution does not exceed 28°C to avoid premature production of vitamin D during the photochemical reaction. 3 . The reaction was monitored by high pressure liquid chromatography (HPLC) (Instrument: ...

Embodiment 2

[0040] (1) Light response of 7-dehydrocholesterol

[0041] 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 is mixed evenly with magnetic stirring to prepare a photochemical reaction solution. The reaction liquid was placed in an internal immersion photochemical reactor that had placed a 450-watt high-pressure mercury lamp (same as Example 1) and was venting nitrogen. Adjust the flow of nitrogen to make the bubbles uniform. Start the mercury lamp and count it. The reaction device is placed in an opaque fume hood, and an electric fan is added to ensure that the temperature of the photochemical reaction solution does not exceed 28°C to avoid premature production of vitamin D during the photochemical reaction. 3 . The reaction was monitored by high pressure liquid chromatography (HPLC) (the conditions were the same as in Example 1), and the reaction was c...

Embodiment 3

[0049] (1) Light response of 7-dehydrocholesterol

[0050] 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, and add 10 mg of 2,6-di-tert-butyl The base-p-methoxyphenol is uniformly mixed with magnetic stirring to prepare a photochemical reaction solution. The reaction liquid was placed in an internal immersion photochemical reactor that had placed a 450-watt high-pressure mercury lamp (same as Example 1) and was venting nitrogen. Adjust the flow of nitrogen to make the bubbles uniform. Start the mercury lamp and count it. The reaction device is placed in an opaque fume hood, and an electric fan is added to ensure that the temperature of the photochemical reaction solution does not exceed 28°C to avoid premature production of vitamin D during the photochemical reaction. 3 . The reaction was monitored by high pressure liquid chromatography (HPLC) (the conditions were the same as in Example 1), and the react...

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Abstract

The invention belongs to the field of organic photochemical synthesis, in particular to a method for photochemical synthesis of vitamin D3. Under the protection of nitrogen, dissolve 7-dehydrocholesterol in a non-polar-polar solvent mixed system, add antioxidant, stir evenly, and light, control the temperature of the photochemical reaction solution at 23-30°C; evaporate to dryness To the reaction solution, add a polar solvent to separate unreacted 7-dehydrocholesterol from the reaction product; add maleic anhydride with a molar ratio of 1.5:1-2:1 to tachysterol under stirring, and a concentration of 45-55wt % KOH or NaOH aqueous solution, get the viscous product that removes tachysterol; measure the content of pre-vitamin D3 and vitamin D3, dissolve in 8-10 times the weight of refined oil, and heat to 60-70 °C under vacuum to remove Vacuum to get clear and high-quality vitamin D3 oil. The invention can increase the yield of vitamin D3 oil to about 70%, and the production process is very simple.

Description

Technical field [0001] The invention belongs to the field of organic photochemical synthesis, and particularly relates to photochemical synthesis of vitamin D 3 Methods. Background technique [0002] Vitamin D 3 It is one of the important vitamins necessary for human health, the normal growth and reproduction of livestock and poultry, and it needs to be added in appropriate amounts 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 both domestically and internationally. At present, only a few countries such as Germany and Switzerland produce them in the world, which are 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℃, the concentration of the reaction raw materials does not exceed 2%, and the conversion rate is 100%. Many by-products requir...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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