Method for purifying 24-dehydrocholesterol

A technology for dehydrocholesterol and compound, applied in the direction of organic chemistry, steroids, etc., can solve the problems of large solvent consumption, high cost, complicated process, etc., and achieve the effects of being conducive to industrialization, low environmental pressure, and simple process
CN113135972AActive Publication Date: 2021-07-20江西天新药业股份有限公司
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Patent Information

Authority / Receiving Office
CN · China
Current Assignee / Owner
江西天新药业股份有限公司
Publication Date
2021-07-20

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Abstract

The invention relates to the technical field of purification of intermediates, in particular to a method for purifying 24-dehydrocholesterol, which comprises the following steps: (1) taking a mixture containing a compound as shown in a formula (I) and a compound as shown in a formula (II) as a raw material to be purified, and obtaining a first purified product in a mode of step (1A) or (1B); (1A) in the presence of a first solvent, contacting the raw material to be purified with MXn to obtain a complex, and then decomplexing in the presence of water and a second solvent; (1B) carrying out column chromatography separation on the raw material to be purified; (2) crystallizing the first purified product by using a third solvent to obtain a second purified product, wherein R in the formula (I) and R in the formula (II) are the same and are H or C1-C4 acyl groups. The method provided by the invention has the advantages of low cost, simple technical process and capability of effectively purifying 24-dehydrocholesterol.
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Description

technical field

[0001] The invention relates to the technical field of intermediate purification, in particular to a method for purifying 24-dehydrocholesterol. Background technique

[0002] 24-dehydrocholesterol or its derivatives are important raw materials for the synthesis of 25-hydroxycholesterol, and 25-hydroxycholesterol is an important raw material for the synthesis of 25-hydroxyvitamin D3. 25-Hydroxyvitamin D3 has wide application prospects and high economic value. But at present, 24-dehydrocholesterol or its derivatives face the problem of difficult purification. Existing methods for purifying 24-dehydrocholesterol generally include the following:

[0003] Method (a) The lanolin cholesterol crystallization liquid material passes through the industrial preparation column (J.Nat.Prod.1996,59,23-26), needs 400-1000 times of elution solvent, solvent consumption is large, energy consumption is high, environmental protection pressure Large, and the high-efficiency sil...

Claims

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