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Method for preparing cefotiam hexetil hydrochloride

A technology of cefotiam and cefotiam, which is applied in the field of drug antibiotics and can solve the problems of increasing crystallization loss and increasing separation processes, etc.

Inactive Publication Date: 2012-07-25
国药集团致君(苏州)制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The introduction of solids such as activated carbon increases the separation process in industrial production and increases crystallization loss

Method used

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0067] (1) Add 600L of acetonitrile and 140Kg of pre-dried NaI to the reaction tank, heat to 50°C under stirring, add 130L of 1-chloroethylcyclohexyl carbonate, and react for 100min. After the reaction was completed, it was concentrated to dryness under reduced pressure at room temperature. CH 2 Cl 2 600L and Na 2 S 2 o 3 Aqueous solution (5%) 400L mixed solvent washes concentrate, collects organic layer, obtains the CH of 1-iodide ethyl cyclohexyl carbonate 2 Cl 2 solution.

[0068] (2) Add KHCO to the reaction tank 3 100Kg, water 30L, acetone 60L and stir to dissolve. Then cefotiam 130Kg was added and stirred at 28°C for 40min. Add 1400L of acetone and stir to dissolve, then cool to 0°C, let stand to separate layers and collect the lower layer, then add DMA600L, stir and dissolve at 25°C to obtain cefotiam salt solution.

[0069] (3) CH of 1-iodoethyl cyclohexyl carbonate 2 Cl 2 The solution was added to the cefotiam salt solution and stirred for reaction at a te...

Embodiment 2

[0075] (1) Add 600L of acetonitrile and 140Kg of pre-dried NaI to the reaction tank, heat to 50°C under stirring, add 130L of 1-chloroethylcyclohexyl carbonate, and react for 100min. After the reaction was completed, it was concentrated to dryness under reduced pressure at room temperature. CH 2 Cl 2 600L and Na 2 S 2 o 3 Aqueous solution (5%) 400L mixed solvent washes concentrate, collects organic layer, obtains the CH of 1-iodide ethyl cyclohexyl carbonate 2 Cl 2 solution.

[0076] (2) Add KHCO in the reaction tank 3 100Kg, water 30L, acetone 60L and stir to dissolve. Then cefotiam 130Kg was added and stirred at 28°C for 40min. Add 1700L of acetone and stir to dissolve, then cool to 0°C, let stand to separate layers and collect the lower layer, then add DMA600L, stir and dissolve at 25°C to obtain cefotiam salt solution.

[0077] (3) CH of 1-iodoethyl cyclohexyl carbonate 2 Cl 2 The solution was added to the cefotiam salt solution and stirred for reaction at a temp...

Embodiment 3

[0083] (1) Add 600L of acetonitrile and 140Kg of pre-dried NaI to the reaction tank, heat to 50°C under stirring, add 130L of 1-chloroethylcyclohexyl carbonate, and react for 100min. After the reaction was completed, it was concentrated to dryness under reduced pressure at room temperature. CH 2 Cl 2 600L and Na 2 S 2 o 3 Aqueous solution (5%) 400L mixed solvent washes concentrate, collects organic layer, obtains the CH of 1-iodide ethyl cyclohexyl carbonate 2 Cl 2 solution.

[0084] (2) Add KHCO to the reaction tank 3 100Kg, water 30L, acetone 60L and stir to dissolve. Then cefotiam 130Kg was added and stirred at 28°C for 40min. Add 1700L of acetone and stir to dissolve, then cool to 0°C, let stand to separate layers and collect the lower layer, then add DMA600L, stir and dissolve at 25°C to obtain cefotiam salt solution.

[0085] (3) CH of 1-iodoethyl cyclohexyl carbonate 2 Cl 2 The solution was added to the cefotiam salt solution and stirred for reaction at a te...

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Abstract

The invention discloses a method for preparing and purifying cefotiam salt and cefotiam hexetil hydrochloride. The method comprises the following steps of: reacting cefotiam with bicarbonate to prepare cefotiam salt; and reacting the prepared and purified 1-iodoethyl cyclohexyl carbonate with the cefotiam salt to prepare the cefotiam hexetil. The cefotiam hexetil hydrochloride is prepared by performing hydrochloric acidification and purification on the cefotiam hexetil. The method for preparing the cefotiam hexetil hydrochloride has a simple preparation process, at the purification part, the extraction is combined with crystallization by using a mixed solvent, and meanwhile, a water-soluble reducing agent is added in a step of easily changing color, so that the finished product of high purity, high yield and good color is obtained. The cefotiam hexetil hydrochloride prepared by the method of the invention has the purity of over 98.5 percent and the yield of over 95 percent.

Description

technical field [0001] The invention relates to the preparation of cefotiam axetil, in particular to a method for preparing and purifying cefotiam axetil hydrochloride, which belongs to the field of drug antibiotics. Background technique [0002] Cefotiam (CTM) is a second-generation cephalosporin, its structural formula is shown in formula (I), cefotiam esterification can obtain cefotiam hexetil (Cefotiam hexetil), its structural formula is shown in formula (II). [0003] [0004] Cefotiam can be made into oral antibiotics. The oral antibiotics themselves have no antibacterial effect. After oral administration, they are quickly hydrolyzed into cefotiam in the intestinal mucosa and absorbed. Cefotiam has the same antibacterial activity against Gram-positive and negative bacteria as The cephalosporins orally administered in the past are the same, and they are stable to β-lactamase. They are effective against clinically isolated Staphylococcus aureus, coagulase-negative sta...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D501/36C07D501/04C07D501/12
Inventor 史利军孙元强潘一凯赵申喆
Owner 国药集团致君(苏州)制药有限公司
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