Method for sensitized preparation of cis-vitamin D or its derivs. using cross-linked polymer photosensitizer

A technology of cross-linking polymers and photosensitizers, applied in the direction of organic chemistry, can solve problems such as co-precipitation of raw materials and products with photosensitizers, inability to separate azeotropes, environmental protection issues, etc., to prevent mutual quenching and dimerization The effect of avoiding mutual contact and prolonging the service life

Inactive Publication Date: 2003-10-29
TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to improve this technology, Clarke E. Slemon (EP0 252 740/1988) invented a soluble polymer photosensitizer and used it to convert the toxic by-product tachysterol generated in vitamin D production into pre-vitamin D photosensitizer Firstly, the polymer photosensitizer and the reaction substrate are dissolved in the solvent, and the photosensitive isomerization reaction is carried out by light. After the reaction, a precipitant is added to precipitate the polymer photosensitizer, and then the sensitizer and the reaction substrate are filtered and washed. Product separation, although this method saves the column chromatography separation process, the product will be included during the precipitation of the polymer photosensitizer, and some products will co-precipitate with the polymer photosensitizer. The primary dissolution and precipitation process uses a large amount of solvents, and the recovered mixed solvents must be purified and

Method used

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Examples

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Example Embodiment

[0019] The specific embodiment embodiment 1. take Merrifield resin as the synthesis of the cross-linked macromolecular photosensitizer of skeleton

[0022] 5 milliliters of toluene, 3 milliliters of methyl methacrylate, 0.3 milliliters of divinylbenzene, 141.7 milligrams of anthracene methyl methacrylate and 38.8 milligrams of benzoyl peroxide were put into the polymerization reactor, and nitrogen gas was passed for 40 minutes to remove the system Oxygen in the reaction at 80 ℃ for 24 hours. The obtained polymer was pulverized and washed successively with ethyl acetate, ethanol, diethyl ether and petroleum ether until there was no anthracene in the washing solution. The obtained polymer was put into a vacuum oven and dried at 50° C. for 12 hours. The content of the calibrated anthracene chromophore in the cross-linked polymer is 6×10 -5 Moore G -1 . This cross-linked polymer photosensitizer is called PMMA-An. Embodiment 3. take Merrifield resin as the ...

Example Embodiment

[0019] The specific embodiment embodiment 1. take Merrifield resin as the synthesis of the cross-linked macromolecular photosensitizer of skeleton

[0023] Add 1.0 g of chloromethylated polystyrene with a crosslinking degree of 1%, a particle size of 200-400 mesh, and a chlorination rate of 2.0-2.5 mmol / g in 30 ml of dry N, N-dimethylformamide Resin (Merrifield resin), protected from light and heated to reflux, was added with 0.69 g (1.0 mmol) and 1.38 g (2.0 mmol) of eosin disodium salt respectively. The reaction was stopped after reflux in the dark for 22 hours, allowed to stand at room temperature, and filtered with suction. The filtrate was washed successively twice with 100 ml of toluene, ethanol, ethanol-water (1:1), water, water-ethanol (1:1), and 100 ml of ethanol. A bright orange fine powder is finally obtained. After vacuum drying, two cross-linked polymer photosensitizers with eosin functional groups but with different loading rates were obtain...

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Abstract

A process for preparing cis-vitamine D or its derivative by use of cross-linked high-molecular photosensitizer includes dissolving trans-vitamind D or its derivative in solvent, adding said photosensitizer, sensitizing reaction under light irradiation, filtering and washing. Its advantages are simple purifying separation, and less consumption of sensitizer.

Description

technical field [0001] The invention belongs to the field of synthesizing vitamin D and its derivatives by photochemical method, and particularly relates to a method for sensitizing and preparing cis-vitamin D or its derivatives with a cross-linked polymer photosensitizer. Background technique [0002] The photoisomerization reaction of trans-vitamin D and its derivatives is an important step in the synthesis of active vitamin D. Trans-vitamin D or its derivatives are converted into cis-vitamin D or its derivatives in the presence of photosensitizers, such as active vitamin D 2 and D 3 . [0003] A large number of studies have shown that in the presence of suitable photosensitizers, trans-vitamin D or its derivatives can be converted into cis-vitamin D or its derivatives through photoisomerization reaction, and the toxic by-product tachysterol generated in the production of vitamin D Can be converted to pre-vitamin D. [0004] Organic small molecule ...

Claims

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Application Information

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IPC IPC(8): C07C401/00
Inventor 李嫕高云燕游长江谢蓉陈金平刘白宁韩永滨
Owner TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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