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Preparation process of ticarcillin disodium salt

A technology of ticarcillin disodium salt and ticarcillin acid, which is applied in organic chemistry and other fields, and can solve problems such as high pH, ​​high impurity content, and high water content

Active Publication Date: 2009-05-13
ZHUHAI UNITED LAB
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

There are obvious shortcomings and deficiencies in the freeze-drying method: the crystal form of the product produced by the freeze-drying method is poor; The role of impurities, high impurity content; due to the presence of other salts, the pH is high, the stability of the product is poor, and there are disadvantages of high cost and high equipment investment
[0007] The slurry method of GB131145 also has prominent shortcomings, that is, it needs to adopt temperature-programmed crystallization method in slurry liquid, which will lead to product degradation, increase of impurities and decrease of stability
[0008] GB1449749 adopts methyl isobutyl ketone and dichloromethane to extract, directly add the methyl isobutyl ketone solution of sodium isooctanoate to precipitate the product, and the HPLC purity is 85% in terms of ticarcillinic acid, but this method is easy A mixture of monosodium salt and disodium salt is precipitated, resulting in unqualified pH value of the product and demanding operation

Method used

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  • Preparation process of ticarcillin disodium salt
  • Preparation process of ticarcillin disodium salt

Examples

Experimental program
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Effect test

Embodiment 1

[0033] At 0°C, extract the reaction solution containing 50g of ticarcillinic acid twice with 50mL×2 butyl acetate, combine the butyl acetate extracts, dilute with 50mL of acetone, add 2g of activated carbon, decolorize for 30min, filter, and Add an acetone solution of sodium isooctanoate to the mother liquor, add seed crystals, stir and grow the crystals at 10°C for 2.5 hours, then slowly add 100mL of acetone, after the addition is complete, filter under reduced pressure, and dry in vacuum at 80°C to obtain white ticarcillin disodium Salt, yield 78%; 1 HNMR(D2O): 7.44(m, 1H), 7.34(m, 1H), 7.13(m, 1H), 5.58(d, 1H), 5.47(d, 1H), 4.68(m, 1H), 4.24(m , 1H), 1.5(m, 6H).

Embodiment 2

[0035] At 50°C, extract the reaction solution containing 10 g of ticarcillinic acid twice with 10 mL×2 butyl acetate, combine the butyl acetate extracts, dilute with 50 mL of butyl acetate, add 0.5 g of activated carbon, and decolorize for 30 min. Filtrate, add sodium isocaproate acetone solution to the mother liquor, add seed crystals, stir and grow crystals at 5°C for 2.5h, then slowly add 500mL of acetone, after addition, filter under reduced pressure, vacuum dry at 40°C to obtain white ticar Cillin disodium salt, HPLC purity 99.1%, maximum impurity 0.4%.

Embodiment 3

[0037] At -5°C, extract the reaction solution containing 5g ticarcillinic acid twice with 10mL×2 dichloromethane, combine the dichloromethane extracts, dilute with 10mL methanol, add 0.2g activated carbon, decolorize for 30min, and filter , add methanol solution of sodium methoxide to the mother liquor, add seed crystals, stir and grow the crystals at 10°C for 2.5h, then slowly add 500mL of acetone, after the addition is complete, filter under reduced pressure, and vacuum dry at 20°C to obtain white ticarcillin di Sodium salt, HPLC purity 99.0%, maximum impurity 0.3%.

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Abstract

The invention discloses a making method of penicillin antibiotic disodium tikaxilin salt, which comprises the following steps: adding diluent in the tikaxilin acid solution at -5-50 deg. c; decoloring through active carbon; filtering; adding salting agent; stirring; culturing crystal at -10-50 deg. c until the crystal is evolved completely; filtering; washing; drying in the vacuum under 20-80 deg. c; obtaining the product.

Description

technical field [0001] The invention relates to the field of pharmaceutical products, in particular to a method for preparing various penicillin antibiotics ticarcillin disodium salts. technical background [0002] Ticarcillin is a semi-synthetic penicillin. It was first listed in Japan. It is a penicillin with a new structure and is particularly effective for severe Gram-negative bacterial infections. Its common preparation is Ticarcillin Sodium / Clavulanic Potassium for Injection. Its antibacterial spectrum is similar to that of carbenicillin. But its antibacterial activity against Pseudomonas aeruginosa is 2 to 4 times that of carbenicillin. Relatively low activity against Gram-positive bacteria, but high activity against Gram-negative bacteria. Compound preparations of ticarcillin sodium and clavulanate potassium are often used clinically, and the combination of the two not only expands the antibacterial spectrum, but also enhances the antibacterial activity. So as to...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D499/70
Inventor 阙灵刘毓宏唐彬喜左斌海
Owner ZHUHAI UNITED LAB
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