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Green high-efficiency synthetic method for doxycycline hydrochloride

A doxycycline hydrochloride, high-efficiency technology, applied in chemical instruments and methods, preparation of organic compounds, preparation of sulfonates, etc., can solve the problems of high cost, low yield, poor stereoselectivity, etc., and achieve green and simple. Effect

Inactive Publication Date: 2018-08-24
HENAN NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

After experimental comparison, it is found that if the heterogeneous Pd / C is used as the catalyst in the one-step method, the stereoselectivity is poor and the yield is low; the silica gel-bonded Rh(PPh 3 ) 3 Although Cl is a homogeneous catalyst, the cost is high; and the two-step method in the literature has the disadvantage of low yield

Method used

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  • Green high-efficiency synthetic method for doxycycline hydrochloride
  • Green high-efficiency synthetic method for doxycycline hydrochloride
  • Green high-efficiency synthetic method for doxycycline hydrochloride

Examples

Experimental program
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Effect test

Embodiment 1

[0022] Put 1.5g of palladium chloride powder into a beaker containing 250mL of deionized water, fully dissolve it to obtain a palladium chloride solution for use; weigh 4g of sodium hydroxide and put it into a beaker containing 50mL of deionized water, fully Stir to obtain a sodium hydroxide solution for use; add 3.0 g of eicosenoic acid to the beaker of the prepared sodium hydroxide solution, and place the beaker in an ultrasonic cleaner and stir vigorously to fully dissolve the eicosenoic acid until Sodium eicosenoate solution is obtained until there is no massive eicosenoic acid in the solution; heat the prepared 250mL palladium chloride solution to 65°C, and then quickly add the prepared eicosenoic acid solution while stirring the palladium chloride solution Palladium hydroxide solution can be obtained by adding sodium acrylate solution, and the palladium hydroxide solution is continuously stirred for 10 minutes to make the reaction more uniform; 100 mL of hydrogen peroxide...

Embodiment 2

[0024] Put 1.5g of palladium chloride powder into a beaker containing 250mL of deionized water, fully dissolve it to obtain a palladium chloride solution for use; weigh 4g of sodium hydroxide and put it into a beaker containing 50mL of deionized water, fully Stir to obtain a sodium hydroxide solution for use; add 3.0 g of eicosatrienoic acid to the beaker of the prepared sodium hydroxide solution, and place the beaker in an ultrasonic cleaner and stir vigorously to fully dissolve the eicosatrienoic acid , until there is no massive eicosatrienoic acid in the solution to obtain sodium eicosatrienoate solution; heat the prepared 250mL palladium chloride solution to 65°C, and then quickly add the prepared palladium chloride solution while stirring eicosatrienoic acid sodium solution, palladium hydroxide solution can be obtained, keep stirring for 10min to make the reaction more uniform; add 100mL mass concentration of 30% hydrogen peroxide solution to the obtained palladium hydroxi...

Embodiment 3

[0026] Put 1.5g of palladium chloride powder into a beaker containing 250mL of deionized water, fully dissolve it to obtain a palladium chloride solution for use; weigh 4g of sodium hydroxide and put it into a beaker containing 50mL of deionized water, fully Stir to obtain a sodium hydroxide solution for use; add 3.0 g of linoleic acid to the beaker of the prepared sodium hydroxide solution, and place the beaker in an ultrasonic cleaner and stir vigorously to fully dissolve the linoleic acid until there is no lump in the solution The sodium linoleate solution is obtained until the linoleic acid is like linoleic acid; the prepared 250mL palladium chloride solution is heated to 65°C, and then the prepared sodium linoleate solution is quickly added while stirring the palladium chloride solution to obtain the hydroxide Palladium solution, keep stirring for 10min to make the reaction more uniform; add 100mL of hydrogen peroxide solution with a mass concentration of 30% in the obtain...

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Abstract

The invention discloses a green high-efficiency synthetic method for doxycycline hydrochloride, and belongs to the technical field of medicine synthesis. A key point of a technical scheme of the invention is that the green high-efficiency synthetic method for the doxycycline hydrochloride has a specific synthetic route shown in the description. The method disclosed by the invention has the advantages that the synthetic method is green and simple, raw materials are cheap and easy to obtain, and a yield of the target product is higher.

Description

technical field [0001] The invention belongs to the technical field of pharmaceutical synthesis, and in particular relates to a green and efficient method for synthesizing doxycycline hydrochloride. Background technique [0002] The chemical name of Doxycycline Hydrochloride is 6-methyl-4-(dimethylamino)-3,5,10,12,12α-pentahydroxy-1,11-dioxo-1,4 ,4α,5,5α,6,11,12α-octahydro-2-tetracenecarboxamide hydrochloride hemiethanol hemihydrate is a classic semi-synthetic tetracycline antibiotic with broad-spectrum, potent and long-acting specialty. Doxycycline hydrochloride is not only a human medicine, but also widely used in forestry, animal husbandry and fishery. In addition, studies have shown that doxycycline hydrochloride also has various pharmacological activities such as anti-tumor and neuroprotection. [0003] At present, the synthesis of doxycycline hydrochloride mostly uses oxytetracycline as a raw material, and first obtains a mixture of 11α-chloro-6,12-hemiketal oxytetr...

Claims

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Application Information

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IPC IPC(8): C07C231/12C07C237/26
CPCC07C231/12C07C303/32C07C2603/46C07C237/26C07C309/60
Inventor 徐桂清周应杰王家豪毛龙飞姜玉钦李伟
Owner HENAN NORMAL UNIV
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