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Synthetic process of ceftazidime intermediate

A technology of ceftazidime and synthesis process, applied in the field of synthesis technology of ceftazidime intermediates, can solve the problems of low yield, difficult post-processing, long synthesis steps and the like, and achieve the effects of simple synthesis and easy post-processing

Inactive Publication Date: 2012-05-16
许婧
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Benefits of technology

This patented technology makes it easier for scientists to make things that are more efficient than existing methods or techniques used by others.

Problems solved by technology

The technical problem addressed in this patents relating to improving the production process of chemical compounds containing an ester group at position 4 (Ceftrazide) involves finding ways to improve the purity and yields of certain substances that contain a carboxylic acid moiety such as hydroxypropyltrimethylene carbonate (HPTMC).

Method used

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  • Synthetic process of ceftazidime intermediate
  • Synthetic process of ceftazidime intermediate
  • Synthetic process of ceftazidime intermediate

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Embodiment Construction

[0014] The synthesis steps of the present invention are: add 35-40 g of the compound ceftazime side-chain acid ethyl ester to a four-necked flask equipped with a condenser tube and mechanical stirring, the reaction solvent is a mixed solvent of methanol and water, and the volume ratio is V 甲醇 :V 水 =3:1~1:3, add NaOH, m 头孢他啶侧链酸乙酯 :m NaOH =1:1~1:2, stir and react at 15~60°C for 8h; track the reaction with TLC; after the end, add 2g of activated carbon and stir for 1h, filter out insoluble matter; cool the filtrate to 20°C, adjust until the pH is 7; distill under reduced pressure at 40-45°C to recover methanol, dissolve the residue in 75ml of water, adjust the pH to 3 with 1mol / L hydrochloric acid; cool down to 5°C, continue stirring for 30min, filter with suction, and water 50mL in turn 1. Wash the filter cake with 50 ml of acetonitrile, and dry in vacuo to obtain a pale yellow solid.

[0015] The present invention selects solvent composition, alkali consumption, reaction tem...

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Abstract

A synthetic process of a ceftazidime intermediate belongs to the technical field of medicaments, and more particularly, relates to a synthetic process of a ceftazidime intermediate. The invention provides a synthetic process of a ceftazidime intermediate, which is simple, short in time consumption, and high in yield. The synthetic steps of the invention comprise: adding compound ceftazidime side chain acid ethyl ester in a four-mouth bottle equipped with a condenser tube and a mechanical stirrer, wherein the reaction solvent is a mixed solvent of methanol and water with a volume ratio of the methanol and water being 3:1-1:3, adding NaOH with a mass ratio of the ceftazidime side chain acid ethyl ester and NaOH being 1:1-1:2, stirring at 15-60 DEG C; adding 2 g of active carbon, stirring for 1 hour, filtering to remove insoluble substances; cooling the filtrate to 20 DEG C, adjusting the pH to 7 with 1 mol/L hydrochloric acid; performing reduced pressure distillation at 40-45 DEG C to recover methanol, dissolving the residues in 75 ml of water, adjusting the pH to 3 with 1 mol/L hydrochloric acid, performing suction filtration, washing the filter cake by 50 ml of water and 50 ml of acetonitrile in order, performing vacuum drying to obtain a light yellow solid.

Description

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Claims

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Application Information

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Owner 许婧
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