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Method for preparing cefotiam hexetil hydrochloride by cefotiam hydrochloride

A technology of cefotiam axetil hydrochloride and cefotiam hydrochloride, which is applied in the field of medicine, can solve the problems of low yield of cefotiam axetil hydrochloride, low yield of cefotiam salt, unfavorable impurity removal treatment, etc., and achieve High pollution, high purity and low cost

Inactive Publication Date: 2012-09-19
西安万隆制药股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The cefotiam used in this method is unstable under normal conditions, easy to absorb moisture, and cannot be preserved, so it can only be newly prepared for immediate use, which affects the batch industrial production of this product, and will form a gel after directly reacting with acid carbonate It is unfavorable for the de-impurity treatment of the later stage, and acid carbonate is not only reactant in the reaction in addition, but also a kind of catalyst, given cefotiam and acid carbonate (molar ratio 1: 1~ 2) Insufficient consumption of acid carbonate in the proportioning of materials will cause the low yield of cefotiam salt, and then cause the low yield of cefotiam hydrochloride

Method used

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  • Method for preparing cefotiam hexetil hydrochloride by cefotiam hydrochloride
  • Method for preparing cefotiam hexetil hydrochloride by cefotiam hydrochloride
  • Method for preparing cefotiam hexetil hydrochloride by cefotiam hydrochloride

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Embodiment 1

[0038] Embodiment 1: a kind of preparation method of cefotiam hydrochloride comprises following preparation steps:

[0039] ① Add 60ml of water to 100g of KHCO3, stir quickly, and slowly add 120g of cefotiam hydrochloride at 25-30°C, after adding, continue to keep stirring at 25-30°C for 30 minutes. React under reduced pressure for 30-40 minutes, then add 25 times the amount of acetone (water) to the reaction system, lower the temperature to 0°C within 30 minutes, stop stirring, stand still for more than 30 minutes, and transfer The supernatant was obtained as cefotiam potassium salt.

[0040]②Add 550ml of N,N-dimethylformamide preheated to 30-40°C to cefotiam potassium salt, and stir the mixed system under reduced pressure below 30°C for 1 hour to dissolve the potassium salt. After dissolving, cool down to - 15~-20°C, add 1-iodide ethyl cyclohexyl carbonate which is pre-cooled to below -15°C into the reaction system, control the temperature at -15~-20°C and stir for 30 minut...

Embodiment 2

[0047] Embodiment 2: a kind of preparation method of cefotiam hydrochloride comprises following preparation steps:

[0048] ①Add 30ml of water and 60ml of acetone to 380g of NaHCO, stir rapidly, slowly add 100g of cefotiam hydrochloride at 25-30°C, react under reduced pressure for 30-40 minutes, then add fifty times (water ) amount of acetone, the temperature was lowered to 0~-5°C within 30 minutes, the agitation was stopped, the stratification was static for more than 30 minutes, and the supernatant was removed to obtain cefotiam sodium salt.

[0049] ②Add 500ml of N,N-dimethylacetamide preheated to 30-35°C to cefotiam sodium salt, and stir the mixed system under reduced pressure below 35°C for 1.5 hours to dissolve the sodium salt, then cool down to - 15~-20℃, add 1-iodide ethyl cyclohexyl carbonate which has been pre-cooled to below -15℃ into the reaction system, control the temperature at -5~-10℃ and stir for 25 minutes, then add and cool down to 2℃ The following 3500ml o...

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Abstract

The invention discloses a method for preparing cefotiam hexetil hydrochloride by cefotiam hydrochloride, belonging to medicines. The method comprises the steps of leading the cefotiam hydrochloride and potassium bicarbonate or sodium bicarbonate to react to prepare cefotiam, wherein the cefotiam hydrochloride is produced in an industrialized scale manner andthe charging mol ratio of the cefotiam hydrochloride and potassium bicarbonate or sodium bicarbonate is 1:2.5-10; then reacting with carbonic acid 1-iodinated cyclohexyl ethyl ester to obtain cefotiam hexetil; and conducting purification and hydrochloric acid acidization to obtain cefotiam hexetil hydrochloride. According to the method, especially the cefotiam is prepared by reacting cefotiam hydrochloride with 2.5-10 times of mol ratio of potassium bicarbonate or sodium bicarbonate in water, the prepared cefotiam hexetil hydrochloride has high purity, the total quantity of related substances in the prepared product is smaller than 1.5% by adopting a HPLC (high performance liquid chromatograp) method for detection, the yield rate is larger than 90%, and the production cost is low, thus being beneficial to industrialized manufacturing.

Description

technical field [0001] The invention relates to a method for preparing cefotiam axetil hydrochloride with cefotiam hydrochloride, in particular to a method for preparing cefotiam salt in water with cefotiam hydrochloride and potassium bicarbonate or sodium bicarbonate having a molar ratio of 2.5 to 10 times. Pharmaceutical field. Background technique [0002] Cefotiam hydrochloride is the second-generation cephalosporin. Cefotiam hydrochloride for injection has been produced by many domestic companies and imported from abroad. It has been widely used clinically. Its structural formula is as shown in formula (I). Cefotiam hydrochloride becomes potassium salt or sodium salt, react with 1-iodoethyl cyclohexyl carbonate, and then purify and hydrochloride to obtain cefotiam hydrochloride, whose structural formula is shown in formula (II). [0003] [0004] The active body of this product is cefotiam, which is hydrolyzed and converted into cefotiam in the intestinal tract afte...

Claims

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Application Information

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IPC IPC(8): C07D501/04C07D501/36
Inventor 陈婧
Owner 西安万隆制药股份有限公司
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