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A kind of purification method of 7-dehydrocholesterol leftovers

A technology of dehydrocholesterol and purification method, which is applied in the field of purification of 7-dehydrocholesterol leftovers, can solve the problems of large solvent and energy consumption, environmental pollution, use, etc., and achieves high industrial feasibility, simple reaction process, and realization The effect of economic benefits

Active Publication Date: 2019-01-29
SICHUAN YUXIN PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] About 10% of 7-dehydrocholesterol is contained in the scraps of 7-dehydrocholesterol in the production process, and this part of 7-dehydrocholesterol accounts for about 20% of the total production of 7-dehydrocholesterol. Due to the large amount of 3- The presence of hydroxycholesta-4,6-diene and other scraps prevents 7-dehydrocholesterol scraps from being used in industrial production and discarded, causing vitamin D 3 The production cost is high and pollutes the environment
This method can separate and obtain 7-dehydrocholesterol products with higher purity, and the process is simple, which has certain application value, but at the same time, there are disadvantages such as small processing capacity, low recovery rate, large solvent and energy consumption, and difficulty in reusing the adsorbent.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Add 500ml of cyclohexane to 100.5g of 7-dehydrocholesterol scraps containing 10.2g of 7-dehydrocholesterol, heat up to 50°C to dissolve, and make a raw material solution with a concentration of 10g / ml; mix the raw material solution with an equal volume of sulfolane Mix evenly, oscillate in a constant temperature oscillator at 200r / min for 3h, and then stand at constant temperature for 2h. The extract of the upper layer was concentrated at a temperature of 40°C and a pressure of 0.095Mpa to 1 / 5 of the total amount of the original extract; the concentrated product was frozen and crystallized at a temperature of -20°C for 10 hours and then filtered to obtain purified 7-de Hydrocholesterol.

Embodiment 2

[0025] Add 450ml of cyclohexane to 95g of 7-dehydrocholesterol scrap containing 8.7g of 7-dehydrocholesterol, heat up to 40°C for dissolution, and make a raw material solution with a concentration of 15g / ml; mix the raw material solution with an equal volume of N- Mix the methylpyrrolidone evenly, shake it in a constant temperature oscillator at 250r / min for 3h, and then let it stand at constant temperature for 2h. The extract of the upper layer was concentrated at a temperature of 30°C and a pressure of 0.09Mpa to 1 / 5 of the total amount of the original extract; the concentrated product was frozen and crystallized at a temperature of -20°C for 10 hours, and then filtered to obtain purified 7-de Hydrocholesterol.

Embodiment 3

[0027] Add 310ml of cyclohexane to 50g of 7-dehydrocholesterol scrap containing 3.6g of 7-dehydrocholesterol, heat up to 45°C to dissolve, and make a raw material solution with a concentration of 20g / ml; mix the raw material solution with an equal volume of N, N-dimethylformamide was mixed evenly, shaken in a constant temperature oscillator at 250r / min for 3h, and then stood at constant temperature for 2h. The extract of the upper layer was concentrated at a temperature of 30°C and a pressure of 0.09Mpa to 1 / 6 of the total amount of the original extract; the concentrated product was frozen and crystallized at a temperature of -20°C for 10 hours, and then filtered to obtain purified 7-de Hydrocholesterol.

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Abstract

The invention discloses a purification method of a 7-dehydrocholesterol waste material. The method comprises the steps of: at 30-50DEG C, mixing the 7-dehydrocholesterol waste material containing the by-product 3-hydroxycholest-4, 6-diene with cyclohexane till complete dissolution to prepare a raw material solution with a concentration of 1-50g / ml; employing an organic solvent to conduct fractional extraction on the raw material solution, collecting the extracted solution and conducting pressure reduced concentration, and then using ethyl acetate to perform crystallization, thus obtaining purified 7-dehydrocholesterol. The purification method of the 7-dehydrocholesterol waste material provided by the invention has the advantages of simple reaction process, no need of excess reaction steps, strong operability, and high industrial feasibility, can really convert the 7-dehydrocholesterol in the waste material into a pure illumination raw material, thereby realizing change of waste into treasure, and realizing economic benefits while solving waste material pollution.

Description

technical field [0001] The invention relates to the field of fine chemicals, in particular to a method for purifying 7-dehydrocholesterol leftovers. Background technique [0002] 7-Dehydrocholesterol for the production of vitamin D 3 It is an important intermediate of cholesterol, which is generally obtained from cholesterol through acylation, oxidation, hydrazone, dehydrazone, and soap cholesterification. In the process of preparing 7-dehydrogenation by the synthetic method, many by-products will be produced due to different debromination selectivities 3 -Hydroxycholesta-4,6-diene, the by-product and 7-dehydrocholesterol are isomers, in the refining process of 7-dehydrocholesterol, it is difficult to separate by physical methods and will lead to a large amount of 7-dehydrocholesterol The loss of dehydrocholesterol, in order to improve the yield of 7-dehydrocholesterol refining, and at the same time completely solve the impact of the existence of 3-hydroxycholesta-4,6-diene...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J9/00
CPCC07J9/00
Inventor 冷莉
Owner SICHUAN YUXIN PHARM CO LTD