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Preparation method of vitamin D

A vitamin and solution technology, applied in organic chemistry methods, organic chemistry and other directions, can solve the problems of hidden dangers in production safety, high energy consumption, and high equipment costs, and achieve the effects of improving yield, reducing costs, and high utilization of raw materials

Inactive Publication Date: 2020-05-08
宁波东隆智能科技有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, most domestic manufacturers of vitamin D industrially use high-power ultraviolet mercury lamps imported from Germany for the light reaction of a single light source. The main defects of this method are ① high cost of equipment used in production; ② high-power lamps cause hidden dangers in production safety and High energy consumption; ③Single light source light reaction has low conversion yield and many impurities
[0005] The Chinese invention patent application with application number CN200880013359.5 (announcement number is CN101668739A) relates to a photochemical method for preparing provitamin D or its derivatives from 7-dehydrosterol or its corresponding derivatives. The method includes: using UV Light irradiates the 7-dehydrosterol or its derivatives until the maximum conversion rate of 7-dehydrosterol or its derivatives is less than 12%. The method of D has lower energy consumption and is safer, but the yield of vitamin D obtained by the photochemical method for preparing pre-vitamin D or its derivatives is low

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0042] 1 g of ergosterol and 80 mL of tetrahydrofuran were evenly mixed to obtain solution A. Under the temperature condition of 10-15°C, the solution A was first irradiated with an LED ultraviolet lamp of the model DL-UVC-UV254-30W for 270 minutes, and the solution B was obtained after the irradiation. Under the temperature condition of 10-15°C, the solution B was irradiated with an LED ultraviolet lamp of the model DL-UVA-UV365-40W for 270 minutes, and the solution C was obtained after the irradiation. Distill the solution C under reduced pressure to remove the solvent, add methanol to cool down and stir for crystallization, stir and crystallize at -20°C to -30°C for 24 hours, and recover the filter cake and filtrate by suction filtration. Ergosterol 95% 0.45g, filtrate pre-vitamin D 2 and vitamin D 2mixture. The filtrate was incubated at 65°C for 8h, then at 30-35°C for 48h, concentrated under reduced pressure to dryness to obtain 0.52g (wherein pre-vitamin D 2 8% Vitam...

Embodiment 2

[0044] Mix 1 g of 7-dehydrocholesterol and 100 mL of tetrahydrofuran uniformly to obtain solution A. Under the temperature condition of 10-15°C, the solution A was first irradiated with an LED ultraviolet lamp of the model DL-UVC-UV254-30W for 300 minutes, and the solution B was obtained after the irradiation. Under the temperature condition of 10-15°C, the solution B was irradiated with an LED ultraviolet lamp of the model DL-UVA-UV365-40W for 300 minutes, and solution C was obtained after the irradiation. Distill the solution C under reduced pressure to remove the solvent, add methanol to cool down and stir for crystallization, stir and crystallize at -20°C to -30°C for 24 hours, and recover the filter cake and filtrate by suction filtration. 95% 7-Dehydrocholesterol 0.43g, filtrate pre-vitamin D 3 and vitamin D 3 mixture. The filtrate was incubated at 65°C for 8h, then at 30-35°C for 48h, concentrated under reduced pressure to dryness to obtain 0.54g (wherein pre-vitamin...

Embodiment 3

[0046] 1 g of 22,23-dehydroergosterol and 60 mL of tetrahydrofuran were uniformly mixed to obtain solution A. Under the temperature condition of 10-15°C, the solution A was irradiated with the LED ultraviolet lamp of the model DL-UVC-UV254-30W for 240 minutes, and the solution B was obtained after the irradiation. Under the temperature condition of 10-15°C, the solution B was irradiated with an LED ultraviolet lamp of the model DL-UVA-UV365-40W for 240 minutes, and the solution C was obtained after the irradiation. Distill the solution C under reduced pressure to remove the solvent, add methanol to cool down and stir for crystallization, stir and crystallize at -20°C to -30°C for 24 hours, and recover the filter cake and filtrate by suction filtration. 22,23-Dehydroergosterol 95% 0.45g, filtrate pre-vitamin D 4 and vitamin D 4 mixture. The filtrate was incubated at a temperature of 65°C for 8h, then at a temperature of 30-35°C for 48h, and concentrated to dryness under redu...

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Abstract

The invention discloses a preparation method of vitamin D. The preparation method is characterized in that the method comprises the following steps: dissolving provitamin D in an organic solvent to obtain a solution as a raw material, and carrying out a two-step photocatalytic reaction process, separating and purifying to obtain the vitamin D, wherein the provitamin D is 7-dehydrocholesterol, ergosterol, 22, 23-dehydroergosterol, 7-dehydro-beta-sitosterol, 7-dehydro-stigmasterol or 7-dehydro-campesterol, a lamp used in the first-step photocatalytic reaction is an LED ultraviolet lamp with thewavelength range of 250-260nm, and the lamp used in the second-step photocatalytic reaction is an LED ultraviolet lamp with the wavelength range of 350-380nm. The preparation method of the vitamin D is high in yield.

Description

technical field [0001] The invention relates to the technical field of vitamin D, in particular to a preparation method of vitamin D. Background technique [0002] Vitamin D (vitamin D) is a sterol derivative obtained from different provitamin D after ultraviolet irradiation. Vitamin D is a fat-soluble vitamin, and vitamin D is one of the most important vitamins in the human body. Its main function is to promote the absorption of calcium and phosphorus by intestinal mucosal cells, thereby preventing rickets, promoting the growth and differentiation of skin cells, and regulating immune function. . [0003] Members of the vitamin D family include vitamin D 2 、D 3 、D 4 、D 5 、D 6 、D 7 , among which, the most important member of vitamin D family members is vitamin D 2 (ergocalciferol) and vitamin D 3 (cholecalciferol). Pre-vitamin D is an intermediate of vitamin D, and the one-to-one correspondence of the above-mentioned vitamin D is pre-vitamin D 2 、D 3 、D 4 、D 5 、...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C401/00
CPCC07B2200/07C07C401/00C07C2601/14C07C2602/24
Inventor 郑坚应园
Owner 宁波东隆智能科技有限公司
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