A kind of preparation and purification method of aldehyde oil methanol solution

A methanol solution and purification method technology, applied in the preparation of imino compounds, organic chemistry, etc., can solve the problems of increasing the production cost of sulfadiazine products, not involving purification methods, affecting the safety of medication, etc., to improve labor productivity and reduce impurities , the effect of quality improvement

Active Publication Date: 2020-04-03
JILIN BEISHA PHARMA
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0003] At present, the aldehyde oil methanol solution is directly diluted and used without purification, and there are many impurities in it. When the sulfadiazine product is synthesized, the quality of the product is directly affected by the introduction of impurities, and the production cost of the sulfadiazine product is increased, which in turn affects the safety of its medication
[0004] CN1034719A (1989-08-16) discloses a method for producing sulfadiazine, but this process does not involve a specific purification method, and its preparation process is also quite different from the present invention

Method used

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  • A kind of preparation and purification method of aldehyde oil methanol solution
  • A kind of preparation and purification method of aldehyde oil methanol solution
  • A kind of preparation and purification method of aldehyde oil methanol solution

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Embodiment 1

[0028] Ingredients: 340kg of vinyl ether, 306kg of dimethylformamide, 323kg of phosphorus trichloride, 1360kg of kerosene, 850kg of anhydrous methanol, 510kg of petroleum ether;

[0029] In a 3000L glass-lined addition reactor, add 1360kg of kerosene, turn on the chilled water to cool down to 29℃, add 91.8kg of dimethylformamide into the addition reactor, the temperature of the material rises to 40℃; after the addition, continue to cool to At 38°C, the remaining 214.2kg of dimethylformamide and 96.9kg of phosphorus trichloride were added dropwise at the same time. The process took 45 minutes for the material temperature to be 30-37°C, and the temperature was reduced to 35°C; then the remaining 226.1kg was added dropwise at the same time Phosphorus trichloride and 340kg vinyl ethyl ether, dripping takes 58 minutes, the material temperature during the dripping process is 32-35℃, after the dripping is completed, continue to stir for 10 minutes, the material liquid temperature is 34℃,...

Embodiment 2

[0037] Ingredients: 340kg of vinyl ether, 340kg of dimethylformamide, 357kg of phosphorus trichloride, 1530kg of kerosene, 1020kg of anhydrous methanol, 544kg of petroleum ether;

[0038] In a 3000L glass-lined addition reactor, add 1530kg of kerosene, turn on the chilled water to cool to 30℃, then add 119kg of dimethylformamide to the addition reactor, the material temperature will rise to 42℃; continue after adding Cool down to 38°C, start to add the remaining 221 dimethylformamide and 125kg phosphorus trichloride simultaneously. The dropping takes 50 minutes. The temperature of the materials during the dropping process is 30-38°C and the temperature is reduced to 35°C; then at the same time Add the remaining 232 phosphorus trichloride and 340 vinyl ethyl ether dropwise. The dropping time takes 65 minutes. The material temperature during the dropping process is 32-34°C. After the dropping is completed, continue to stir for 12 minutes. The material liquid temperature is 34°C. Af...

Embodiment 3

[0046] Ingredients: 340kg of vinyl ether, 289kg of dimethylformamide, 306kg of phosphorus trichloride, 1190kg of kerosene, 680kg of anhydrous methanol, 408kg of petroleum ether;

[0047] In a 3000L glass-lined addition reactor, add 1190kg of kerosene, turn on the chilled water to cool down to 28°C, then add 115.6kg of dimethylformamide into the addition kettle, the material temperature rises to 43°C; continue to cool down after the addition is complete When the temperature reaches 38°C, start to add the remaining 173.4kg of dimethylformamide and 122.4kg of phosphorus trichloride simultaneously. The addition takes 40 minutes. The temperature of the materials during the dropping process is 30-38°C and the temperature is reduced to 35°C; Add the remaining 183.6kg phosphorus trichloride and 340kg vinyl ethyl ether. The dripping takes 55 minutes. The material temperature during the dripping process is 32-34℃. After the dripping is completed, continue to stir for 10 minutes. The materia...

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Abstract

The invention relates to a medicinal intermediate and a purification method of the medicinal intermediate, in particular to a method for purifying an aldehyde-oil methanol solution. The aldehyde-oil methanol solution is prepared from ethyl vinyl ether, dimethylformamide and phosphorus trichloride, and a preparation method of the medicinal intermediate comprises the steps of: performing an additionreaction by adopting kerosene as solvent to prepare aldehyde oil, diluting the obtained aldehyde oil with anhydrous methanol, and carrying out extraction and purification with petroleum ether to obtain the medicinal intermediate, i.e., the aldehyde-oil methanol solution. The medicinal intermediate can be applied to the production of chemical raw material sulfadiazine products, wherein the petroleum ether, the kerosene, the ethyl vinyl ether and the anhydrous methanol can be reused after fractional distillation. The preparation method of the medicinal intermediate has the advantages of mild reaction conditions and high product yield, the aldehyde-oil methanol solution is good in quality and high in purity, and the improvement of the quality of the chemical raw material sulfadiazine products is facilitated; since the petroleum ether, the kerosene, the ethyl vinyl ether and the anhydrous methanol can be recycled and reused, material consumption can be reduced, postprocessing of the production of follow-up products can be reduced, and pollution on the environment can be reduced.

Description

Technical field [0001] The invention relates to a method for preparing and purifying pharmaceutical intermediates, in particular to a method for purifying aldehyde oil methanol solution. Background technique [0002] Aldehyde oil methanol solution is an important pharmaceutical and chemical intermediate. It is mainly used for the production of chemical raw material sulfadiazine products. Sulfadiazine is mainly used for the prevention and treatment of meningitis caused by meningococcus, and can also be used for upper respiratory tract. Treatment of infection, otitis media, pain, boils and puerperal fever. Sulfonamides are broad-spectrum antibiotics, but because many common clinical pathogens are resistant to these drugs, they are only used for infections caused by sensitive bacteria and other sensitive pathogenic microorganisms. Therefore, the preparation technology of aldehyde oil methanol solution has attracted much attention. [0003] At present, the methanol solution of aldehy...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C249/02C07C251/30
Inventor 黄升刘斌
Owner JILIN BEISHA PHARMA
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