Method for synthesizing vitamin D3 in segmented and fixed spectrum band manner

A vitamin and spectral band technology, applied in the field of photoreaction, can solve the problems of prone to conformational inversion, low yield, low purity and content, etc., to improve the conversion rate of raw materials and product quality, and improve the dissolved concentration of substrates. Effect

Active Publication Date: 2020-12-22
CHONGQING HONOROAD ANIMAL HEALTH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the synthesis of vitamin D3 is mostly composed of 7-dehydrocholesterol by light, removal of tachysterol, removal of 7-dehydrocholesterol, and thermal isomerization steps. The ring rate is low, only about 30%, and the remaining 70% of 7-dehydrocholesterol must be recovered and illuminated again. On the other hand, the content of tachysterol generated during the illumination process is relatively high, about 10%. Toxic substances must be removed. The main reason for impurities is that the light source uses high-pressure mercury lamps. High-pressure mercury lamps will generate a lot of heat and have a wide band.
At the same time, in the process of thermal isomerization, if the control conditions are not good, the conformational reversal of vitamin D3 will easily occur, and trans-vitamin D3 will be generated. The whole process is complicated, the yield is not high, and the purity and content are low.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] (1) Dissolution of 7-dehydrocholesterol

[0019] In the batching kettle, add 237.5kg methanol, 712.5kg n-hexane, add 50kg 7-dehydrocholesterol (content: 96%) under stirring, add 1kg 2,6-tert-butyl p-cresol, stir and heat up to 30°C , to dissolve it;

[0020] (2) First-level fixed-band illumination

[0021] Firstly, pass the first-level fixed-band ultraviolet lamp (the light source is a 10KW LED lamp, wavelength: 290nm) through nitrogen for 30 minutes, turn it on, and preheat it for 30 minutes. Then filter the solution in step (1), pass it through a rotameter and a temperature control device, and pass it into a first-order fixed-spectrum band ultraviolet lamp to control the material flow rate to 400L / hr, control the material inlet temperature to 32°C, and the outlet temperature to 18°C. ℃;

[0022] (3) Second-level fixed-band illumination

[0023] First, pass nitrogen gas through the secondary fixed-band ultraviolet lamp (15KW LED lamp, wavelength: 250nm) for 25 minu...

Embodiment 2

[0027] (1) Dissolution of 7-dehydrocholesterol

[0028] In the batching kettle, add 135.7kg isopropanol, 542.8kg isoheptane, add 50kg 7-dehydrocholesterol (content: 97%) under stirring, add 0.5kg 2,6-tert-butyl p-methylphenol, stir Raise the temperature to 28°C to dissolve it;

[0029] (2) First-level fixed-band illumination

[0030] First pass the first-level fixed-spectrum ultraviolet lamp (the light source is an 8KW LED lamp, wavelength: 300nm) through nitrogen for 25 minutes, turn it on, and preheat it for 20 minutes, then filter the solution in step (1), and pass it through the rotameter and The temperature control device is connected to a first-level fixed-spectrum band ultraviolet lamp to control the material flow rate to 500L / hr, and to control the material inlet temperature to 33°C and the outlet temperature to 20°C;

[0031] (3) Second-level fixed-band illumination

[0032] First, pass the nitrogen gas through the secondary fixed-spectrum ultraviolet lamp (18KW LE...

Embodiment 3

[0036] (1) Dissolution of 7-dehydrocholesterol

[0037] In the batching kettle, add 127.2kg of absolute ethanol, 763.4kg of isopentane, add 75kg of 7-dehydrocholesterol (content: 98%) under stirring, add 2,6-tert-butyl-p-methoxyphenol, stir and heat up to 32°C to make it dissolve;

[0038] (2) First-level fixed-band illumination

[0039] First pass the first-level fixed-spectrum ultraviolet lamp (15KW LED lamp, wavelength: 320nm) with nitrogen gas for 28 minutes, turn it on, and preheat it for 25 minutes, then filter the solution in step (1), and pass it through the rotameter and The temperature control device is connected to a first-level fixed-spectrum band ultraviolet lamp to control the material flow rate to 420L / hr, and to control the material inlet temperature to 29°C and the outlet temperature to 18°C;

[0040] (3) Second-level fixed-band illumination

[0041] First pass the nitrogen gas through the secondary fixed-spectrum ultraviolet lamp (the light source is a 15K...

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PUM

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Abstract

The invention relates to the field of photoreaction, in particular to a method for synthesizing vitamin D3 in a segmented and fixed spectrum band mode. Through segmented illumination, 7-dehydrocholesterol is converted into pre-vitamin D3, and then the pre-vitamin D3 is directly converted into vitamin D3, so that the generation of trans-vitamin D3 is reduced. Meanwhile, an ultraviolet lamp of the photoreactor is fixed at a certain wavelength, and the condition of photoreaction is controlled, so that the conversion rate of converting the 7-dehydrocholesterol into the previtamin D3 is increased to 98 percent, and the generation of impurities such as tachysterol and leucterol is reduced. The method mainly comprises the steps of dissolution, illumination and distillation, the synthesis steps ofVD3 are easier to operate, the quality is easier to control, and industrial production is easier.

Description

technical field [0001] The invention relates to the field of photoreactions, in particular to a method for synthesizing vitamin D3 with segmental fixed bands. Background technique [0002] Vitamin D3 (also known as cholecalciferol) is a drug with antirickets activity, which is widely considered to be an important substance regulating calcium and phosphorus metabolism. Before vitamin D3 was discovered, rickets (also known as rickets) was one of the important diseases that plagued human health. The substance can be transformed into an effective anti-chondrosis active substance after being illuminated. In the early 1930s, scientists Waddel and Windous confirmed that the anti-chondrosis active ingredient in the human body is cholecalciferol produced by 7-DHC light, named vitamin D3. [0003] At present, the synthesis of vitamin D3 is mostly composed of 7-dehydrocholesterol by light, removal of tachysterol, removal of 7-dehydrocholesterol, and thermal isomerization steps. The ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C401/00
CPCC07C401/00C07C2601/14C07C2602/24
Inventor 王国勤赵德任敏
Owner CHONGQING HONOROAD ANIMAL HEALTH
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