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A kind of preparation method of sulfa-6-methoxypyrimidine

A technology of methoxypyrimidine and sodium methoxypyrimidine, which is applied in the field of preparation of sulfonamide-6-methoxypyrimidine, can solve the problems of skin corrosion, irritation of human mucous membranes, uncertainty, etc. Impurities, the effect of environmental protection

Active Publication Date: 2017-11-21
浜田智子
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantages of this method are: firstly, when the calcium salt method is used for refining, it is necessary to add milk of lime to adjust the pH value of the system, and the impurity content of domestic calcium hydroxide is difficult to control, and it is easy to introduce uncertain impurities, thus affecting the refined product. The quality of sulfonamide-6-methoxypyrimidine is affected; secondly, the dust or suspension droplets of calcium hydroxide can irritate the human mucous membrane, which can cause sneezing and coughing. At the same time, it is highly alkaline and corrosive to skin and fabrics , which is not conducive to the protection of laborers; again, there is a large amount of calcium salt in the wastewater after sulfa-6-methoxypyrimidine is refined, which is not conducive to wastewater treatment and environmental protection
Finally, the refined sulfa-6-methoxypyrimidine product has a yellowish appearance, which is difficult to meet the requirements of the Pharmacopoeia (CPV2010)

Method used

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  • A kind of preparation method of sulfa-6-methoxypyrimidine
  • A kind of preparation method of sulfa-6-methoxypyrimidine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Add 85.0 g of crude sulfa-6-methoxypyrimidine sodium, 400 ml of ultrapure water, and 3.5 g of activated carbon into a 1000 ml four-necked round-bottomed flask. The mixture is stirred at 40° C. for 30 minutes and then filtered while hot. The filtrate was transferred to a new 1000 ml four-neck round bottom flask, 5.5 ml of 25% ammonia water and 12.0 g of ammonium sulfate were added, and after distillation for 45 minutes at 60°C (vacuum degree was -0.076~-0.080MPa), the temperature was raised to 95°C , Distilled under the vacuum degree of -0.010~-0.012MPa until there is no obvious ammonia smell. After the distillation is over, add 5% sulfuric acid solution while it is hot until the pH of the reaction system is 5.8, cool down to 45°C and filter, wash the filter cake with ultrapure water and dry it at 85-90°C with a vacuum of -0.093--0.100MPa A white solid of sulfa-6-methoxypyrimidine was obtained.

Embodiment 2

[0018] Add 85.0 g of crude sulfa-6-methoxypyrimidine sodium, 400 ml of ultrapure water, and 3.5 g of activated carbon into a 1000 ml four-necked round-bottomed flask. The mixture is stirred at 40° C. for 30 minutes and then filtered while hot. The filtrate was transferred to a new 1000 ml four-neck round bottom flask, 5.5 ml of 25% ammonia water and 12.0 g of ammonium sulfate were added, and after distillation for 45 minutes at 60°C (vacuum degree was -0.076~-0.080MPa), the temperature was raised to 95°C , Distilled under the vacuum degree of -0.010~-0.012MPa until there is no obvious ammonia smell. After the distillation is over, add 5% sulfuric acid solution while it is hot until the pH of the reaction system is 6.0, cool down to 45°C and filter, wash the filter cake with ultra-pure water and dry it at 85-90°C with a vacuum of -0.093--0.100MPa A white solid of sulfa-6-methoxypyrimidine was obtained.

Embodiment 3

[0020] Add 85.0 g of crude sulfa-6-methoxypyrimidine sodium, 400 ml of ultrapure water, and 3.5 g of activated carbon into a 1000 ml four-necked round-bottomed flask. The mixture is stirred at 40° C. for 30 minutes and then filtered while hot. The filtrate was transferred to a new 1000 ml four-neck round bottom flask, 5.5 ml of 25% ammonia water and 12.0 g of ammonium sulfate were added, and after distillation for 45 minutes at 60°C (vacuum degree was -0.076~-0.080MPa), the temperature was raised to 95°C , Distilled under the vacuum degree of -0.010~-0.012MPa until there is no obvious ammonia smell. After the distillation is over, add 5% sulfuric acid solution while it is hot until the pH of the reaction system is 6.1, cool down to 45°C and filter, wash the filter cake with ultrapure water and dry it at 85-90°C with a vacuum of -0.093--0.100MPa A white solid of sulfa-6-methoxypyrimidine was obtained.

[0021] Repeat the experimental steps described in Example 1 above, changin...

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Abstract

The present invention discloses a preparation method for sulfanilamide-6-methoxypyrimidine. The method comprises the specific steps of: dissolving a sulfanilamide-6-methoxypyrimidine odium crude product in water; after decolorijng and filtering the solution by activated carbon, adding ammonium water and solid ammonium sulfate into the filtrate; carrying out decompressed distillation to no ammoniacal odor is available; then adjusting the pH value to 4-7 by sulfuric acid; and then reducing the temperature, crystallizing, washing and drying the solution to obtain a sulfanilamide-6-methoxypyrimidine pure product. The preparation method provided by the present invention utilizes the property of ammonium sulfate thermal decomposition; and simultaneously at a reduced pressure, the pH value of a reaction system can be smoothly lowered by removing the added ammonium water and ammonia generated after the ammonium sulfate thermal decomposition step by step, so that sulfanilamide-6-methoxypyrimidine can be slowly separated out, and is difficult to pack with impurities; meanwhile, the ammonia by removed by decompression can be absorbed by using the sulfuric acid solution; and ammonium sulfate formed can be recycled and used, so that environmental protection is facilitated.

Description

technical field [0001] The invention belongs to the field of organic chemistry and relates to a preparation method of sulfonamide-6-methoxypyrimidine. Background technique [0002] Sulfa-6-methoxypyrimidine (2), also known as antibacterial sulfonate (synonym DS-36 or SMM), is a long-acting sulfonamide drug, mainly used for the prevention and treatment of hemolytic streptococcus, pneumococcus and meningococcus Infect. Treat coccidiosis, urinary tract and respiratory tract infections and other diseases, and can also be used as feed additives to obtain antibacterial agents. The sulfa-6-methoxypyrimidine recorded in the eighth edition of the Japanese Pharmacopoeia is a hydrate, while the domestically produced ones are all anhydrous, and its structural formula is: [0003] [0004] According to literature reports, such as Chinese Patent Application No. CN 93101799, CN 93106077, the current domestic method for synthesizing sulfa-6-methoxypyrimidine is mainly to use sulfa-6-ch...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D239/69
CPCC07D239/69
Inventor 浜田申一浜田智子汪艺宁郭晓野常永凯陈艳卫文均
Owner 浜田智子
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