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Improved preparation method of penicillin hydriodate

A technology of sacillin hydroiodide and sacillin citrate is applied in the field of preparation of sacillin hydroiodide, which can solve the problems of poor product stability, storage of unfavorable product purification intermediates and control of impurities, etc. , to achieve the effect of easy storage and transportation, easy separation and purification, and avoid concentration operation

Active Publication Date: 2021-10-12
内蒙古联邦动保药品有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method is unfavorable for the purification of products, the storage of intermediates and the control of impurities due to the adoption of a one-pot method, and the use of a more polar acid, the stability of the product is not good

Method used

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  • Improved preparation method of penicillin hydriodate
  • Improved preparation method of penicillin hydriodate
  • Improved preparation method of penicillin hydriodate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] In a 250ml beaker, add 40.0g of water, cool down to 10°C, add 25.0g of β-chlorotriethylamine hydrochloride, stir to dissolve; take another 250ml beaker, add 37.5g of water and 21.0g of potassium carbonate, stir until completely Dissolve; drop the prepared potassium carbonate solution into the chlorinated triethylamine hydrochloride solution, raise the temperature to 20°C, let stand for 1 hour, separate layers, and the upper organic phase is β-chlorinated triethylamine.

[0050] Take a 500ml three-neck flask, add the above organic phase, 200.0g acetone, 40.0g penicillin potassium, stir evenly, heat up to reflux, and react for 4 hours; filter to remove impurities, wash the filter cake with 80.0g acetone, combine the organic phases, add 22.38g citric acid , grow the crystal for 2 hours; filter, wash the filter cake with 12.36g of acetone, and drain it, and dry the solid at 40°C to obtain 66.61g of sacillin citrate. The yield was 99.1%, and the purity was 99.95% through HPL...

Embodiment 2

[0054] Take a 1000ml beaker, add 50.0g of sacillin citrate, stir and dissolve it with 550g of water at 40°C, filter it into a three-necked flask for later use; dissolve 18g of sodium iodide dihydrate in 25g of water, filter and set aside;

[0055] The temperature in the temperature-controlled three-neck flask is 0°C, the stirring speed is 200 rpm, and the sodium iodide solution is slowly added to the citrate system. Dry at 40°C to constant weight (7 hours) to obtain 40.92 g of sacillin hydroiodide. The yield is 90.4%, and the purity is 99.86% according to HPLC detection and analysis, and the maximum single impurity is less than 0.1%.

Embodiment 3

[0057] Take a 1000ml beaker, add 550g of water, heat up to 20°C, add 50.0g of sacillin citrate, stir to dissolve, filter into a three-necked bottle for later use; dissolve 20g of sodium iodide dihydrate in 28g of purified water, filter, and wait use;

[0058] The temperature in the temperature-controlled three-necked flask is 3°C, the stirring speed is 200 rpm, and the sodium iodide solution is slowly added to the citrate system. After the addition is completed, the crystal is grown for 1.5 hours; Dry at 20°C to constant weight (7 hours) to obtain 40.12 g of sacillin hydroiodide. The yield is 88.9%, and the purity is 99.75% through HPLC detection and analysis, and the maximum single impurity is less than 0.1%.

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Abstract

The invention relates to the field of pharmacy, and particularly provides an improved preparation method of penicillin hydriodate, which comprises the following steps: 1) dissolving penicillin citrate with water, then adding a sodium iodide or potassium iodide solution for reaction, growing crystals, filtering, washing and drying to obtain the penicillin hydriodate. The method disclosed by the invention has the advantages of high yield, easiness in operation and small toxicity, the reaction condition is mild, the product purification, intermediate storage and impurity control are facilitated, and the penicillin hydriodate product with good stability is obtained.

Description

technical field [0001] The invention relates to the field of pharmacy, in particular to an improved preparation method of sacillin hydroiodide. Background technique [0002] Sacillin is a new type of penicillin antibiotic drug, which mainly treats mastitis in dairy cows. Compared with traditional antibiotics or chemical drugs, sacillin has less toxic and side effects, significant curative effect, and low residue compared with other similar products. Many advantages, it is a special antibiotic drug for animals. Sacillin was first developed by the United Kingdom, and was first approved for marketing in August 1999. It is currently on the market in dozens of foreign countries and is widely used, and has achieved good curative effect. The preparation method of sacillin hydroiodide salt reported abroad mainly comprises as follows at present: [0003] DE1014114 discloses a kind of synthetic method of penicillin ester, wherein the method comprises reacting penicillin potassium or...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D499/46C07D499/14C07D499/08C07C59/265C07C51/41
CPCC07D499/46C07D499/14C07D499/08C07C51/412C07C59/265
Inventor 刘红池胡宪明石创业李德乐尹邦志
Owner 内蒙古联邦动保药品有限公司
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