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Preparation method of estrone

A technology of estrone and ketal, which is applied in the field of preparation of estrone, can solve the problems of shortage of raw material resources, long reaction steps, and low biotransformation yield, and achieve a wide range of raw material sources, high total yield, and low cost Effect

Active Publication Date: 2015-10-28
ZHEJIANG XIANJU JUNYE PHARM CO LTD +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0012] The invention proposes a preparation method of estrone, which solves the problems of shortage of raw material resources, long reaction steps and low biotransformation yield in the prior art

Method used

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  • Preparation method of estrone
  • Preparation method of estrone
  • Preparation method of estrone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Mix 10 grams of ADD, 14 milliliters of ethylene glycol, 6 milliliters of triethyl orthoformate, and 100 milliliters of chloroform, stir well and add 0.2 grams of PTS. Under the protection of nitrogen, keep the reaction at 15°C for 16 hours, remove the sample for detection (mobile phase: benzene: acetone = 4:1), add triethylamine and stir for 30 minutes after the reaction is completed. Control the vacuum degree above 0.08MPa, concentrate under reduced pressure to a paste, slowly add water under stirring, continue to concentrate to an internal temperature above 70°C, continue to slowly add water, lower the temperature to 5-10°C, filter, rinse the filter cake with water, and dry it in hot air Dry in a circulating oven to obtain a yellow ketal product with a yield of 112% and a content of 99.2%.

[0045] Put 100 ml of tetrahydrofuran, 10 g of diphenylmethane, and 20 g of biphenyl into a glass flask, stir evenly, blow nitrogen, add 2 g of lithium metal, the reaction is exoth...

Embodiment 2

[0048] Mix 20 grams of ADD, 22 milliliters of ethylene glycol, 18 milliliters of triethyl orthoformate, and 200 milliliters of chloroform, stir well and add 0.4 grams of PTS. Under the protection of nitrogen, keep the reaction at 10°C for 15 hours, remove the sample for detection (mobile phase: benzene: acetone = 4:1), add pyridine and stir for 30 minutes after the reaction is completed. Control the vacuum at 0.1MPa, concentrate under reduced pressure to a paste, slowly add water under stirring, continue to concentrate to an internal temperature of 60°C, continue to slowly add water, lower the temperature to 5°C, filter, rinse the filter cake with water, and dry at 60°C to obtain a yellow color The ketal product has a yield of 110% and a content of 98.9%.

[0049] Put 100 milliliters of dichloromethane, 16 grams of diphenylmethane, and 40 grams of biphenyl into the glass flask, stir evenly, ventilate nitrogen, add 4.0 grams of metal lithium, the reaction is exothermic, the tem...

Embodiment 3

[0052] Mix 20 grams of ADD, 34 milliliters of ethylene glycol, 24 milliliters of triethyl orthoformate, and 200 milliliters of chloroform, stir well and add 0.5 grams of PTS. Under the protection of nitrogen, keep warm at 30°C for 20 hours, remove the sample for detection (mobile phase: benzene: acetone = 4:1), add pyridine and stir for 30 minutes after the reaction is completed. Control the vacuum at 0.1MPa, concentrate under reduced pressure to a paste, slowly add water under stirring, continue to concentrate to an internal temperature of 65°C, continue to slowly add water, lower the temperature to 10°C, filter, rinse the filter cake with water, and dry at 60°C to obtain a yellow color The ketal product has a yield of 113% and a content of 99.1%.

[0053] Put 100 milliliters of chloroform, 18 grams of diphenylmethane, and 38 grams of biphenyl into the glass flask, stir evenly, ventilate nitrogen, add 4.0 grams of metal lithium, the reaction is exothermic, the temperature is ...

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Abstract

The invention proposes a preparation method of estrone. The synthesis process route is shown in the formula (please see the formula in the specification). Leftovers ADD of soybean oil serve as raw materials to replace diene, the estrone is fast synthesized just through two steps of chemical reactions, energy consumption is reduced, pollution is reduced, and the three-waste yield of the method is only 1 / 10 of a traditional technology. Raw material sources are very wide, cost is low, and the preparation method is suitable for industrialized application and popularization. The obtained product is high in total yield. The purity is as high as 99.0% after processing is performed, the any individual impurity is smaller than 0.1%, and the estrone reaches the standard of the United States Pharmacopoeia. The mass yield is 60-65%.

Description

technical field [0001] The invention relates to the technical field of preparation of estrone, in particular to a preparation method of estrone. Background technique [0002] The traditional production route uses dienes as raw materials, and is prepared through 6 steps of chemical reactions, including ketoxime, rearrangement, chloroalcoholization, cyclization, cyclization hydrolysis, ring opening, and biofermentation, and 1 step of biofermentation. The production route is long, the supply of raw materials is exhausted, the yield of the synthesis reaction is low, and highly toxic substances such as phosphorus oxychloride are used. The biological fermentation requires a lot of energy consumption, the conversion yield is low, and a large amount of three wastes are produced. The overall cost of producing estrone is therefore high. [0003] The synthetic route is as follows: [0004] [0005] [0006] At the same time, with the rise of research on sterol resources, there ...

Claims

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Application Information

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IPC IPC(8): C07J1/00
CPCC07J1/0059
Inventor 张峥斌胡明晖
Owner ZHEJIANG XIANJU JUNYE PHARM CO LTD
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