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Preparation method of cefixime side chain acid active ester

A technology of cefixime side chain acid and active ester, which is applied in the field of medicine, can solve the problems of low yield, long reaction time, and low production capacity, and achieve the effects of high product purity, simple operation, and increased yield

Pending Publication Date: 2021-05-25
SHANDONG JINCHENG KERUI CHEMICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The above patents have long reaction time, low production capacity, high energy consumption, low yield, large amount of solvent, environmental protection and cost pressure

Method used

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  • Preparation method of cefixime side chain acid active ester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] At 20°C, add 52g of cefixime side chain acid and 81gDM into a mixed solution of 250ml of dichloroethane and acetonitrile, the mass ratio of acetonitrile to dichloroethane is 1:7, add 7.2ml of triethylamine and 0.4ml of pyridine, lower the temperature to 8°C, add 41ml of triethyl phosphite dropwise, add dropwise for 2.5h, under the stirring condition of 200 rpm, use a microwave reactor, adjust the microwave insulation temperature to 15°C, and the microwave radiation power to 80W, The radiation time is 60min. The temperature was lowered to 3°C, and 68 g of cefixime side-chain acid active ester was obtained by suction filtration, with a yield of 96.57% (calculated as cefixime side-chain acid), a purity of 99.7%, and a content of more than 99.2%.

[0036] The structure of cefixime side chain acid active ester is characterized as follows:

[0037] Elemental analysis (%) measured value (calculated value)

[0038] C47.96 (48.00), H3.98 (4.00), N12.42 (12.44), S21.35 (21.33)....

Embodiment 2

[0040] At 25°C, add 52g of cefixime side chain acid and 81gDM into a mixed solution of 250ml of dichloroethane and acetonitrile, the mass ratio of acetonitrile to dichloroethane is 7:1, add 7.2ml of triethylamine and 0.4ml aniline, cool down to 10°C, add 41ml triethyl phosphite dropwise, add dropwise for 2.5h, under the stirring condition of 600 rpm, use a microwave reactor, adjust the microwave holding temperature to 20°C, and the microwave radiation power to 150W, The radiation time is 40min. The temperature was lowered to -2°C, and 69 g of cefixime side chain acid active ester was obtained by suction filtration, with a yield of 97.89% (based on cefixime side chain acid), a purity of 99.6%, and a content of more than 99.3%.

Embodiment 3

[0042] At 30°C, add 52g of cefixime side chain acid and 81g of DM into a mixed solution of 250ml of dichloroethane and acetonitrile, the mass ratio of acetonitrile to dichloroethane is 1:7, add 7.2mN,N-dichloroethane Methylaniline and 0.4ml aniline, lower the temperature to 15°C, add 41ml triethyl phosphite dropwise, add dropwise for 2.5h, under the stirring condition of 500 rpm, use a microwave reactor, adjust the microwave holding temperature to 25°C, microwave The radiation power is 200W, and the radiation time is 30min. The temperature was lowered to 1° C., and 70 g of cefixime side chain acid active ester was obtained by suction filtration, with a yield of 99.31% (based on cefixime side chain acid), a purity of 99.8%, and a content of more than 99.3%.

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Abstract

The invention belongs to the technical field of medicines, and particularly relates to a preparation method of cefixime side chain acid active ester. Cefixime side chain acid and dibenzothiazyl disulfide are used as raw materials, a mixed solution of dichloroethane and acetonitrile is used as a solvent, triethyl phosphite is dropwise added under the catalysis of a catalyst for a microwave reaction, and the cefixime side chain acid reactive ester is obtained after post-treatment. The method is simple to operate and low in cost, the productivity is greatly improved, the yield is improved, and the product purity is high and reaches 99.6% or above.

Description

technical field [0001] The invention belongs to the technical field of medicine, and in particular relates to a preparation method of cefixime side chain acid active ester. Background technique [0002] Microwave chemistry is a new interdisciplinary subject developed vigorously in the 1990s. Its main content is to use high-frequency microwave energy to change the positive and negative poles of dipole molecules in reactants and solvents at a speed of billions of times per second. Dipole eddy currents, ion conduction and high-frequency friction are generated, and a large amount of heat is generated in a short period of time, thereby promoting various chemical reactions. At present, microwave heating technology is widely used in synthetic chemistry, analytical chemistry, petrochemical industry, mineral metallurgy and other chemical research. However, the severe thermal effect in the microwave heating process is easy to produce a series of side reactions. [0003] Low-temperatu...

Claims

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Application Information

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IPC IPC(8): C07D277/74
CPCC07D277/74
Inventor 房正薇姜启英刘明仁
Owner SHANDONG JINCHENG KERUI CHEMICAL CO LTD
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