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Preparation method of 7-ketone sterides

A compound and ketosteroid technology, which is applied in the field of preparing 7-keto steroids, can solve problems such as serious environmental pollution, and achieve the effects of less dosage, easy availability and mild reaction conditions

Inactive Publication Date: 2014-05-14
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But similarly, when adopting this method, it is still unavoidable to use toxic reagent (for PDC), serious environmental pollution

Method used

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  • Preparation method of 7-ketone sterides
  • Preparation method of 7-ketone sterides
  • Preparation method of 7-ketone sterides

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Embodiment 1, a kind of preparation method of 7-ketocholesterol, carries out following steps successively:

[0039] Add 4.28g (0.01mol) of 3-acetylcholesterol and 1.63g (0.01mol) of NHPI into a three-necked flask, and at the same time add 60mL of acetone. After the 3-acetylcholesterol and NHPI are completely dissolved, add 5.14g ( 0.04mol) of tert-butyl hydroperoxide, while starting to stir, react at 20-25°C for 24h.

[0040] After the reaction, the reaction solution was distilled under reduced pressure (0.09MPa) to a yellow oil, 30mL of n-hexane was added and stirred again, heated to 40°C and stirred for 30 minutes, then cooled to room temperature, filtered, and the filter cake was the catalyst NHPI.

[0041] Distill the filtrate under reduced pressure (0.09MPa) until there is almost no n-hexane, then add 20mL of pyridine and 5mL of acetic anhydride, leave it overnight at room temperature, then distill under reduced pressure (0.09MPa), then add 10mL of methanol, and fi...

Embodiment 2-10

[0044] Change the kind and consumption of catalyst (as shown in table 1), all the other are equal to embodiment 1, obtain embodiment 2~10; The yield of gained product is as shown in table 1 below:

[0045] Table 1

[0046]

Embodiment 11-14

[0048] Change oxidizing agent---consumption and the reaction time of tert-butyl hydroperoxide, all the other are equal to embodiment 1, get embodiment 11~14; The yield of gained product is as shown in table 2 below:

[0049] Table 2

[0050] Example

[0051]

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Abstract

The invention discloses a preparation method of 7-ketone sterides. The preparation method comprises the following steps: 1, firstly, dissolving steroids and an N-hydroxyl derivative as a catalyst in a solvent, then adding an oxidizing agent to generate an allylic oxidation reaction at a temperature of 0-60 DEG C, after the sterides are completely oxidized, ending the reaction, wherein the mol ratio of the sterides to the N-hydroxyl derivative as the catalyst is 1:(0.1-10), and the mol ratio of the sterides to the oxidizing agent is 1:(2-10); 2, drying a solvent in a reaction solution obtained in the step 1 by distillation, and then recovering the N-hydroxyl derivative as the catalyst through normal hexane to obtain the 7-ketone sterides.

Description

technical field [0001] The present invention relates to a method for preparing 7-keto steroids from steroids. Background technique [0002] 7-keto steroids are the precursors of vitamin D drugs, which are widely used in medicine, food, pesticide, chemical industry and other fields, and have high practical value. Vitamin D drugs can promote the absorption of calcium and phosphorus in the intestinal tract, ensure the content of these two elements in body fluids, and promote the normal calcification of bones. , Sustain life and maintain health essential vitamins. Therefore, as important precursors for the synthesis of vitamin D drugs, the synthesis of 7-ketosteroids can largely constrain their production. [0003] The main methods of prior art synthetic 7-keto steroids are as follows: [0004] 1. It is obtained by allylic oxidation using chromium reagent as the oxidant. Commonly used chromium reagents such as Collins reagent, PCC, PDC, Cr(CO) 6 etc. (J.Org.Chem, 1999, 64, 2...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J9/00
Inventor 陈新志赵倩钱超
Owner ZHEJIANG UNIV
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