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Method for purifying 7-dehydrocholesterol leftovers

A technology for dehydrocholesterol and a purification method, which is applied in the field of purification of intermediates, can solve the problems of 7-dehydrocholesterol loss, complicated process and high cost, and achieves the effects of high industrial feasibility, simple reaction process and reduced processing cost.

Active Publication Date: 2011-03-23
ZHEJIANG NHU CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002] 7-Dehydrocholesterol for the production of vitamin D 3 In the process of preparing 7-dehydrogenation by synthetic method, more by-product 3-hydroxycholesta-4,6-diene will be produced due to different debromination selectivity, and this by-product is related to 7-dehydrogenation Cholesterol is an isomer. During the refining process of 7-dehydrocholesterol, it is difficult to separate it by physical methods and will cause a large amount of 7-dehydrocholesterol loss. In order to improve the yield of 7-dehydrocholesterol refining, at the same time thoroughly To solve the influence of the existence of 3-hydroxycholesta-4,6-diene on the refining of 7-dehydrogenation and the purification of subsequent products, how to use a more scientific method to remove 3-hydroxycholesta-4,6-diene At the same time avoiding the loss of 7-dehydrocholesterol as much as possible has become an important issue
[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
[0004] Chinese Patent No. 200610052797.5 discloses a method for preparing 7-dehydrocholesterol, which purifies 7-dehydrocholesterol through a series of chemical reactions and various solvent crystallization methods. higher

Method used

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  • Method for purifying 7-dehydrocholesterol leftovers

Examples

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Embodiment 1

[0019] Example 1: Add 500 ml of methanol into 100.5 g of 7-dehydrocholesterol scrap containing 10.2 g of 7-dehydrocholesterol, heat up to 50° C. for dissolution, and then add Al 2 (SO 4 ) 3 5.1g, after 1 hour of reaction, no 3-hydroxycholesta-4,6-diene was detected, then 200ml of distilled water and 300ml of n-hexane were added and extracted three times, then the silica gel chromatography column was used to obtain the content of 7-dehydrocholesterol 25.8 g of a mixture with a content of 34.5%, and 10.3 g of a mixture with a 7-dehydrocholesterol content of 68.5% were obtained after recrystallization from 10 times the volume of methanol.

Embodiment 2

[0020] Example 2: Add 500 ml of ethanol to 103.2 g of 7-dehydrocholesterol offal containing 11.2 g of 7-dehydrocholesterol, heat up to 35° C. to dissolve, and then add AlCl 3 6.2g, after 35 minutes of reaction, no 3-hydroxycholesta-4,6-diene was detected, then 200ml of distilled water and 300ml of n-hexane were added and extracted three times, then applied to a silica gel chromatography column to obtain a 7-dehydrocholesterol content of 37.6 % of the mixture 26.5g, after 8 times the volume of ethanol recrystallization to obtain 7-dehydrocholesterol content of 72.5% of the mixture 11.5g.

Embodiment 3

[0021] Example 3: 105.5 g of 7-dehydrocholesterol residue containing 10.5 g of 7-dehydrocholesterol was put into 500 ml of ethanol, and after being heated to 45° C. for dissolution, FeCl was put into 3 5.5g, after 50 minutes of reaction, no 3-hydroxycholesta-4,6-diene was detected, then 200ml of distilled water was added, 300ml of n-hexane was fully extracted three times and then applied to a silica gel chromatography column to obtain a 7-dehydrocholesterol content of 35.5 % of the mixture 25.9g, 10.8g of the mixture with a 7-dehydrocholesterol content of 75.2% was obtained after recrystallization from 10 times the volume of methanol.

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Abstract

The invention discloses a method for purifying the intermediate 7-dehydrocholesterol leftovers of vitamin D3, which aims to solve the problem that the 7-dehydrocholesterol leftovers cannot be used and are discarded in industrial production due to the existence of a large amount of 3-hydroxycholestane-4,6-diene and the leftovers thereof to cause the high production cost of the vitamin D3 and environmental pollutions. The method comprises the following steps of: dissolving the 7-dehydrocholesterol leftovers containing the byproduct 3-hydroxycholestane-4,6-diene into an alcohol solvent in a volume which is twice to 10 times the weight of the leftovers, and stirring the mixture until the leftovers are completely dissolved; and adding an iron salt or aluminum salt into the system, continuing to perform stirring until the impurity 3-hydroxycholestane-4,6-diene is completely reacted, performing extraction on the obtained solution by using varsol, and then separating and removing the 3-hydroxycholestane-4,6-diene by using a chromatographic column. In the method, ether impurities produced in the reaction process can be easily separated from 7-dehydrocholesterol, so the treatment process is greatly reduced.

Description

technical field [0001] The present invention relates to the purification of intermediates, specifically a kind of vitamin D 3 The purification method of the intermediate 7-dehydrocholesterol residue. Background technique [0002] 7-Dehydrocholesterol for the production of vitamin D 3 In the process of preparing 7-dehydrogenation by synthetic method, more by-product 3-hydroxycholesta-4,6-diene will be produced due to different debromination selectivity, and this by-product is related to 7-dehydrogenation Cholesterol is an isomer. During the refining process of 7-dehydrocholesterol, it is difficult to separate it by physical methods and will cause a large amount of 7-dehydrocholesterol loss. In order to improve the yield of 7-dehydrocholesterol refining, at the same time thoroughly To solve the influence of the existence of 3-hydroxycholesta-4,6-diene on the refining of 7-dehydrogenation and the purification of subsequent products, how to use a more scientific method to remo...

Claims

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Application Information

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IPC IPC(8): C07J9/00
Inventor 曹家明车来滨
Owner ZHEJIANG NHU CO LTD
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