Method for photochemosynthesis of vitamin D2

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

Inactive Publication Date: 2006-02-15
TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The illumination system involved in these researches is complex, post-processing is troublesome, and it is 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.; ; 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, ergosterol 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
[0005] Another reason that restricts photochemical industrial scale production is the selection of photochemical reactors and light sources.

Method used

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  • Method for photochemosynthesis of vitamin D2
  • Method for photochemosynthesis of vitamin D2
  • Method for photochemosynthesis of vitamin D2

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] (1) Photoresponse of ergosterol

[0040] In a 500-liter batching kettle, at room temperature, 2 kg of ergosterol was dissolved in 100 liters of hexane-ethanol (2:1, V / V) mixed solvent, and 1.4 grams of 2,6-di-tert-butyl- P-methoxyphenol, stir and mix evenly, and configure the photochemical reaction solution. The reaction solution was pumped into a 4 kW high-pressure mercury lamp (product of UV-Consulting Peschl, Germany) and a large-scale photochemical reactor of internal immersion upward bubbling type with nitrogen gas. Adjust the nitrogen flow rate to make the bubbles uniform. Start the mercury lamp. The reaction solution was flowed through the photoreactor at a flow rate of 1.4 liters / minute for illumination. A cold water jacket and shading jacket are added to the reaction device to ensure that the temperature of the photochemical reaction solution does not exceed 28°C to avoid premature formation of vitamin D during the photochemical reaction 2 . The reaction l...

Embodiment 2

[0052] (1) Photoresponse of ergosterol

[0053] In a 500-liter batching kettle, dissolve 2 kilograms of ergosterol in 100 liters of petroleum ether (60-90° C.)-methanol (7:1, V / V) mixed solvent, and add 1.4 grams of 2,6-di-tert-butyl Base-p-methoxyphenol, stir and mix evenly, and configure the photochemical reaction solution. Following process and condition are with embodiment 1.

[0054] (2) reclaim ergosterol

[0055] After the above photochemical reaction was completed, the reaction solution was successively pumped into the kettle of a 50-liter integrated reactor (QVF Compact Reactor), evaporated to dryness under reduced pressure, and the solvent was recovered. An additional 10 liters of methanol was added and frozen overnight at -20°C. The next day, it was quickly centrifuged by a centrifuge (Henkel HF 300) to obtain 1.31 kg of solid ergosterol (which can be used as a raw material for the next photoreaction).

[0056] (3) Thermal isomerization reaction to produce vitam...

Embodiment 3

[0065] (1) Photoresponse of ergosterol

[0066] In a 500-liter batching kettle, dissolve 4 kilograms of ergosterol in 200 liters of hexane-methanol (9:1, V / V) mixed solvent, add 2.4 grams of 2,6-di-tert-butyl-p-cresol , stirred and mixed evenly, and configured into a photochemical reaction solution. The reaction solution is pumped into a 10 kW high-pressure mercury lamp (product of UV-Consulting Peschl, Germany) and nitrogen-filled large-scale photochemical reactor with internal immersion upward bubbling. Adjust the nitrogen flow rate to make the bubbles uniform. Start the mercury lamp. The reaction solution was flowed through the photoreactor at a flow rate of 2.8 liters / minute for illumination. A cold water jacket and shading jacket are added to the reaction device to ensure that the temperature of the photochemical reaction solution does not exceed 28°C to avoid premature formation of vitamin D during the photochemical reaction 2 . The reaction liquid flowed while bein...

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Abstract

The invention relates to a method for photochemosynthesis of vitamin D2, which comprises dissolving lysergol into a mixed system of nonpolar-polar solvent at the presence of nitrogen protection, charging anti-oxidant, controlling temperature of the photochemical reaction solution at 23-30 deg C, guaranteeing high concentration with mixed solvent, controlling conversion rate of the lysergol below 35%, using non-reacted lysergol as the raw material for next photochemical reaction. The process can substantially increase the concentration of the reactants.

Description

technical field [0001] The invention belongs to the field of organic photochemical synthesis, in particular to industrial photochemical synthesis of vitamin D 2 Methods. Background technique [0002] Vitamin D 2 The physiological function in human, livestock and other mammals is mainly to regulate calcium and phosphorus metabolism, promote the absorption of calcium and phosphorus in the intestine, and also promote the absorption of calcium and phosphorus in renal tubules, and maintain the blood calcium and phosphorus in the body. Balance, promote bone calcification and normal development of bones. As a medicine and food additive, it plays an important role in preventing and treating rickets in children and osteoporosis in the elderly. It can also be used in animal husbandry as a feed additive. At the same time, it is also an important raw material for the synthesis of many other drugs such as active vitamin D. With the development of society and the improvement of peopl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C401/00
Inventor 程学新张宝文刘颙颙王雪松
Owner TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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